乙醇 → Ethyl (4-methylbenzylthio)acetate

HRID 477332

反应方程式

HRID 477332 反应方程式
[SH:1][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].CC[O-].[Na+].C(O)C.Br[CH2:16][C:17]1[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=1>ClCCl>[CH3:16][C:17]1[CH:22]=[CH:21][C:20]([CH2:23][S:1][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4])=[CH:19][CH:18]=1

参与物

6

反应物 4

HCID 702乙醇HCID 77214-甲基溴苄HCID 12185巯基乙酸乙酯HCID 2723922乙醇钠

产物 1

HCID 4107274Ethyl (4-methylbenzylthio)acetate

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

Ethyl 2-mercaptoacetate (8.5 cc) is added in the course of 15 minutes at a temperature in the region of 20° C. to a stirred solution, through which a stream of nitrogen is passed, of a 2M ethanolic solution of sodium ethylate (37.5 cc) and ethanol (50 cc). The mixture is left with stirring for 15 minutes at the same temperature, and α-bromo-p-xylene (13.9 g) is then added in the course of 20 minutes at a temperature in the region of 20° C. Stirring is maintained for 60 minutes at this temperature, and the reaction mixture is then evaporated to dryness at 50° C. under reduced pressure (20 mm Hg; 2.7 kPa). The residue obtained is dissolved in dichloromethane (100 cc), and the organic phase is dried over anhydrous magnesium sulphate, filtered and concentrated to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa). Ethyl (4-methylbenzylthio)acetate (15.6 g) is thereby obtained, and is used in the crude state in the subsequent syntheses.

后处理

  1. waitThe mixture is left
  2. additionis then added in the course of 20 minutes at a temperature in the region of 20° C
  3. temperatureis maintained for 60 minutes at this temperature
  4. customthe reaction mixture is then evaporated to dryness at 50° C. under reduced pressure (20 mm Hg; 2.7 kPa)
  5. customThe residue obtained
  6. dry with materialthe organic phase is dried over anhydrous magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa)

来源与证据

ORD记录
ord-5f945fb988944ca2b579be667497689b
来源数据集
uspto-grants-1989_12
专利号
US04886835

关联笔记

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