Water → HCID 21317597, 화합물

HRID 328772노트

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HRID 328772 반응식
Cl[CH2:2][CH2:3][S:4]([CH:7]([CH2:19][CH2:20][CH2:21][CH:22]([O:28]C(=O)C)[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]CC)=[O:15])(=[O:6])=[O:5].[OH-].[Na+].O>O1CCCC1>[CH:3]([S:4]([CH:7]([CH2:19][CH2:20][CH2:21][CH:22]([OH:28])[CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]([OH:16])=[O:15])(=[O:6])=[O:5])=[CH2:2]

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 21317539HCID 21317539, 화합물

생성물 1

HCID 21317597HCID 21317597, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
25 °C

실험 절차

A mixture of ethyl 8-(2-chloroethylsulfonyl)-12-acetoxyheptadecanoate (43.5 g., 0.09 mole), sodium hydroxide (14.4 g., 0.36 mole), water (150 ml.) and tetrahydrofuran (600 ml.) is stirred at 25° C. for 24 hours. Most of the tetrahydrofuran is removed by evaporation in vacuo keeping the temperature of the evaporating solution at 30° C. or below. The residue is diluted with water (300 ml.) and extracted with ether. The aqueous solution is acidified with dilute hydrochloric acid. The oily product is taken up in ether, washed with water and dried over sodium sulfate. The ether is evaporated to leave the product as a yellowish, very viscous oil. Purification is effected by column chromatography on silica gel with benzene-dioxane as eluting solvent mixture. The title compound is obtained as a colorless viscous oil.

후처리

  1. customMost of the tetrahydrofuran is removed by evaporation in vacuo
  2. customat 30° C. or below
  3. additionThe residue is diluted with water (300 ml.)
  4. extractionextracted with ether
  5. washwashed with water
  6. dry with materialdried over sodium sulfate
  7. customThe ether is evaporated
  8. customto leave the product as a yellowish, very viscous oil
  9. customPurification
  10. washas eluting solvent mixture

출처 및 근거

ORD 기록
ord-4753a9d3e9c347e4acf6b685f13ca38c
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04018802

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