2-Mercaptoethanol → HCID 21317600, 화합물

HRID 328769노트

반응식

HRID 328769 반응식
[SH:1][CH2:2][CH2:3][OH:4].[Na].Br[CH:7]([CH2:19][CH2:20][CH2:21][CH:22]([O:28][C:29](=[O:31])[CH3:30])[CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15]>CO>[OH:4][CH2:3][CH2:2][S:1][CH:7]([CH2:19][CH2:20][CH2:21][CH:22]([O:28][C:29](=[O:31])[CH3:30])[CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15]

참가 물질

5

반응물 3

HCID 15672-MercaptoethanolHCID 5360545SodiumHCID 21317595Ethyl 8-bromo-12-acetoxyheptadecanoate

생성물 1

HCID 21317600HCID 21317600, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2-Mercaptoethanol (31.2 g., 0.4 mole) is dissolved in a solution of sodium (9.2 g., 0.4 mole) in methanol (300 ml.). Ethyl 8-bromo-12-acetoxy-heptadecanoate (Example 1, Step E) (43.5 g., 0.1 mole) is added and the resulting solution is heated at reflux for 5 hours. Most of the methanol is then removed by evaporation in vacuo. Water (350 ml.) is added to the residue and the oily product taken up in ether, washed with water and brine and dried over sodium sulfate. Evaporation of the ether leaves the title compound as a yellow residual oil which is used in the next step without further purification.

후처리

  1. temperaturethe resulting solution is heated
  2. temperatureat reflux for 5 hours
  3. customMost of the methanol is then removed by evaporation in vacuo
  4. additionWater (350 ml.) is added to the residue
  5. washwashed with water and brine
  6. dry with materialdried over sodium sulfate
  7. customEvaporation of the ether

출처 및 근거

ORD 기록
ord-17e9edbdcf264740b0293c5731a02758
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04018802

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