2-Thiopheneacetyl chloride → (E,E,E)-7-hydroxymethyl-3,11,15-trimethyl-2,6,10,14-hexadecatetraen-1-ol bis-2-thienylacetate

HRID 26987

반응식

HRID 26987 반응식
[OH:1][CH2:2]/[C:3](/[CH2:12][CH2:13]/[CH:14]=[C:15](\[CH3:22])/[CH2:16][CH2:17][CH:18]=[C:19]([CH3:21])[CH3:20])=[CH:4]/[CH2:5][CH2:6]/[C:7](/[CH3:11])=[CH:8]/[CH2:9][OH:10].[S:23]1[CH:27]=[CH:26][CH:25]=[C:24]1[CH2:28][C:29](Cl)=[O:30]>N1C=CC=CC=1>[S:23]1[CH:27]=[CH:26][CH:25]=[C:24]1[CH:28]([C:24]1[S:23][CH:27]=[CH:26][CH:25]=1)[C:29]([O:10][CH2:9]/[CH:8]=[C:7](\[CH3:11])/[CH2:6][CH2:5]/[CH:4]=[C:3](/[CH2:2][OH:1])\[CH2:12][CH2:13]/[CH:14]=[C:15](\[CH3:22])/[CH2:16][CH2:17][CH:18]=[C:19]([CH3:21])[CH3:20])=[O:30]

참가 물질

4

실험 절차

To a solution of 1.0 g of (E,Z,E) and (E,E,E)-7-hydroxymethyl-3,11,15-trimethyl-2,6,10,14-hexadecatetraen-1-ol in 5 ml of anhydrous pyridine was added dropwise 2 ml of 2-thienylacetyl chloride under ice-cooling. After 1 hour, ice-water was added and extraction was done with ethyl ether. The ether layer was washed successively with dilute hydrochloric acid, aqueous sodium hydrogencarbonate and water and dried over anhydrous sodium sulfate. The solvent was distilled off to give an oily substance, which was then purified by a column chromatography with silica gel (15 g) to afford 1.1 g of the end product.

후처리

  1. temperaturecooling
  2. extractionextraction
  3. washThe ether layer was washed successively with dilute hydrochloric acid, aqueous sodium hydrogencarbonate and water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off
  6. customto give an oily substance, which
  7. customwas then purified by a column chromatography with silica gel (15 g)

출처 및 근거

ORD 기록
ord-ee288c12f09b46149684686f66e16633
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04151357

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