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

HRID 257402

反応式

HRID 257402 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-fb59fbb2420d4eaabb24576be1e36a79
出典データセット
uspto-grants-1993_11
特許番号
US05262086

関連ノート

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