2-Mercaptoethanol → HCID 21317600、化合物

HRID 328769ノート

反応式

HRID 328769 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 21317600HCID 21317600、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-17e9edbdcf264740b0293c5731a02758
出典データセット
uspto-grants-1977_04
特許番号
US04018802

反応ノート

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