Triethylamine → Benzoic acid, 4-(phenylmethoxy)-, 1-(trifluoromethyl)nonyl ester

HRID 257402

반응식

HRID 257402 반응식
[CH2:1]([O:8][C:9]1[CH:17]=[CH:16][C:12]([C:13](Cl)=[O:14])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[F:18][C:19]([F:31])([F:30])[CH:20]([OH:29])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28].CN(C1C=CC=CN=1)C.C(N(CC)CC)C>C(Cl)Cl>[CH2:1]([O:8][C:9]1[CH:17]=[CH:16][C:12]([C:13]([O:29][CH:20]([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:19]([F:18])([F:30])[F:31])=[O:14])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 218852-DimethylaminopyridineHCID 37664104-BenzyloxybenzoylchlorideHCID 38644641,1,1-Trifluorodecan-2-ol

생성물 1

HCID 14745753Benzoic acid, 4-(phenylmethoxy)-, 1-(trifluoromethyl)nonyl ester수율 96.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 4-benzyloxybenzoic acid chloride (1.23 g) in methylene chloride (10 ml) was added by little and little under ice-cooling a solution of optically active 1,1,1-trifluoro-2-decanol (0.96 g), dimethylaminopyridine (0.55 g) and triethylamine (0.48 g) in methylene chloride (20 ml). The mixture was left to stand overnight at room temperature in order to effect a reaction before the mixture obtained was poured in ice-water. Extraction was effected with methylene chloride and the extracted phase was washed with dilute aqueous hydrochloric acid solution, water, 1N aqueous sodium carbonate solution and water in due order before it was dried over anhydrous magnesium sulfate. The solvent was distilled off to obtain a crude product which was purified by toluene/silica from ethanol to obtain the titled compound (1.84 g).

후처리

  1. waitThe mixture was left
  2. customa reaction before the mixture
  3. customobtained
  4. extractionExtraction
  5. washthe extracted phase was washed with dilute aqueous hydrochloric acid solution, water, 1N aqueous sodium carbonate solution and water in due order before it
  6. dry with materialwas dried over anhydrous magnesium sulfate
  7. distillationThe solvent was distilled off
  8. customto obtain a crude product which
  9. customwas purified by toluene/silica from ethanol

출처 및 근거

ORD 기록
ord-fb59fbb2420d4eaabb24576be1e36a79
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05262086

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