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英语翻译Preparation(预聚) of tert-butyl-2-carboxy methyl-(甲基)3-(4-

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英语翻译
Preparation(预聚) of tert-butyl-2-carboxy methyl-(甲基)3-(4-bromophenylthio)(镇静剂硫代苯基) propionate(丙酸脂) (6).to a mixture of naome (13.8g,0.255mol) in methanol(甲醇) (300ml) was added a solution(溶解、溶液) of 4-bromothiophenol(镇静剂苯硫酚) (36.2g,0.19mol) in methanol (400ml).then to this mixture was added dropwise(逐滴地) a solution of compound (化合物)prepared(事先) in step 3 (32g,0.17mol) in methanol(150mol)
准备
The reaction mixture(混合反应物) was stirred overnight (突然搅拌)at room temperature(室温),then concerntrated in vacuo(真空).the residue(残余物) was diluted with (以——稀释)water and washed several times with ether(乙醚).The aqueous phase(水溶液) was cooled (冷却)at 0C,acidified (使——酸化)with 4N HCl and extracted (萃取)several times with ether.The organic pahse (有机相)was dried (干燥)over MgSO4 washed with brine(浓盐水) and concentrated in vacuo.Flash chromatography(套色板)(silica gel(硅胶),20% ethyl acetate(乙酸乙酯) in petroleum ether)(石油醚) of the residue(残余物) gave compound(化合物) 6..(48g,80.2%).H NMR(1氢核磁共振)(200MHz,DMSO-d6(二甲基亚砜-d6)):&(PPM(百万分率)) 12.4 (S,1h; OH),7.6-7.4 (2d,4H,Ph),3.2 (m,2H,CH2S),2.8 (m,1H,CHCO),2.5m,2H,CH2CO2H),1.4(s,9H,tBu).IR:《伊利诺斯研究》 Vmax 2665-2575,1716 cm.
Anal.(C15H19BrO4S):C,H,S calcd:48.01; 5.10; 8.54.Found:48.43; 5.21; 8.83.
Preparation(预聚) of tert-butyl(丁基)-2-(2-hydroxy-ethyl(2-羟基-乙荃)-3-(4-bromophenylthio(4-镇静剂硫化苯基) propionate(丙酸脂) (4).To a mixture(混合物) of compound 6 (48g,0.128mol) in DME (测距装置)(200ml) at 0C was added(额外的) sequentially(连续地) N-methylmorpholine(N-甲基吗啉) (18ml,0.16mol) and isobutylchloroformiate(异丁基氯仿甲酸脂) (22ml,0.16 mol).The reaction mixture(混合反应物) was stirred(搅拌) overnight(迅速) at room temperature and the precipitate(沉淀物) removed by filtration(过滤).To the filtrate(滤出液) was added at -10C a solution(溶解) of NaBH4(7.26g,0.19mol) in water (150ml).after 1h ,the reaction mixture(混合反应物) was diluted(冲淡、稀释) with water (200ml),acidified(使——酸化) with 1N HCl (100ml) and extracted(萃取) with ethyl acetate(乙酸乙酯).The organic phase(有机相) was washed with brine(浓盐水),dried(干燥) over NaSO4 and concentrated(压缩、压缩) in vacuo.Flash chromatography(套色版) (silica gel(硅胶),gradient(变化程度) of ethyl acetate(乙酸乙酯) in petroleum ether(石油醚)) gave compound 4(34g,74%).H NMR(1氢核磁共振) (200MHz,CDCl3):& (ppm百万分率)) 7.4-7.25 (2d,4H,PH),3.7 (q,2H,OCH2),3.25-3.0 (2dd,2H,CH2S),2.65 (q,1H,CHCO),1.9 (m,2H,OCH2CH2),1.6(t,1H,OH),1.45(s,9H,tBu).IR:Vmax 3427,1726cm.(M+) (C15H19O4S79Br):calcd:360.0395.found:360.0378.(C15H19O4S81Br):calcd:362.0375.found:362.0362.
英语翻译Preparation(预聚) of tert-butyl-2-carboxy methyl-(甲基)3-(4-
制备(预聚)叔丁基- 2 -羧甲基- (甲基) 3 -( 4 - br omophenylthio)(镇静剂硫代苯基)丙酸(丙酸脂) ( 6 ) .混合na ome(8月1 3日克,0.255mol )在甲醇(甲醇) (三百毫升)增加了解决方案(溶解,溶液) 4 - bromothiophenol (镇静剂苯硫酚) ( 36.2克,0.19mol )在甲醇( 400毫升) ,然后以这种混合加入滴(逐滴地)的解决方案化合物(化合物)准备(事先)在第3步(三二克,0.17mol )在甲醇( 150mol )
反应混合物(混合反应物)是激起通宵(突然搅拌)在室温下(室温) ,然后concerntrated在真空中(真空) .残留(残余物)稀释(以-稀释)水和洗涤多次醚(乙醚) .水相(水溶液) ,冷却(冷却)在0c ,酸化(使-酸化)与4 n H Cl和提取(萃取)多次与醚.有机pahse (有机相)干(干燥)硫酸镁冲洗盐水(浓盐水)和集中在真空中.闪存色谱法(套色板) (矽胶(硅胶) ,20 %的醋酸乙酯(乙酸乙酯)在石油醚) (石油醚)的残留(残余物)了化合物(化合物) 6 ..(四八克,80.2 % ) .核磁共振氢谱( 1氢核磁共振) ( 200兆赫,二甲基亚砜-在D6 (二甲基亚砜-D 6中) ):&(百万分之一(百万分率) ) 1 2.4( ,1小时;哦) ,7月6日至7月4日(二维,4小时,pH值) ,3.2 (男,2小时,ch2s ) ,2.8 (男,1小时,chco ) ,2.5米,2小时,ch2co2h ) ,1.4 ( ,9h ,tbu ) .红外:“伊利诺斯研究”的Vmax 2665年至2575年,一千七百十六厘米.
肛门.( c15h19bro4s ) :碳,氢,硫calcd :48.01 ; 5.10 ; 8.54 .发现:48.43 ; 5.21 ; 8.83 .
制备(预聚)叔丁基(丁基) -2 -( 2 -羟基乙基(2 -羟基-乙荃)- 3 - ( 4- br o m op henylthio(4-镇静剂硫化苯基)丙酸(丙酸脂) ( 4 ) .一个混合物(混合物)的化合物6 (四八克,0.128mol )在二甲醚(测距装置) ( 200毫升)在0c加入(额外的)顺序(连续地) N -甲基(的N -甲基吗啉) (一十八毫升,0.16mol )和isobutylchloroformiate (异丁基氯仿甲酸脂) ( 22毫升,0.16 mol )时.反应混合物(混合反应物) ,搅拌(搅拌)通宵(迅速)在室温和沉淀(沉淀物)拆除过滤(过滤) .向滤液(滤出液)加在- 10 C的解决方案(溶解)硼氢化钠(七点二六克,0.19mol )在水(一百五十毫升) .1小时后,反应混合物(混合反应物)被摊薄(冲淡,稀释)与水(二〇 〇毫升) ,酸化(使-酸化)与1 N的盐酸( 1 00毫升)和提取(萃取)与醋酸乙酯(乙酸乙酯) .有机相(有机相)洗涤与卤水(浓盐水) ,干(干燥) naso4和集中(压缩,压缩)在真空中.闪存色谱法(套色版) (矽胶(硅胶) ,梯度(变化程度) ,乙酸乙酯(乙酸乙酯)在石油醚(石油醚) )了化合物4 (三四克,74 % ) .核磁共振氢谱( 1氢核磁共振) ( 200 MHz的,cdcl3 ) :& ( ppm的百万分率) ) 7月4日至7月25日(二维,4小时,pH值) ,3.7 (的Q 2小时,och2 ) ,3.25-3.0 ( 2dd ,2小时,ch2s ) ,2.65 (的Q 1 ,chco ) ,1.9 (男,2小时,och2ch2 ) ,1.6 (吨,上半年,哦) ,1.45 ( ,9h ,tbu ) .红外:3427的Vmax ,1726厘米.(米+ ) ( c15h19o4s79br ) :calcd :360.0395 .发现:360.0378 .( c15h19o4s81br ) :calcd :362.0375 .发现:362.0362 .