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Phenoxyethanol → HCID 15670239、化合物

HRID 248698
ノート
印刷プレビュー

反応式

HRID 248698 の反応式
[C:1]([S:4][CH2:5][CH:6]([CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[C:7]([NH:9][C:10]1[CH:11]=[C:12]([CH:19]=[CH:20][CH:21]=1)[C:13]([O:15][CH2:16][C:17]#N)=[O:14])=[O:8])(=[O:3])[CH3:2].[O:29](CCO)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1>CN(C)C1C=CN=CC=1.C(N(CC)CC)C>[C:1]([S:4][CH2:5][CH:6]([CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[C:7]([NH:9][C:10]1[CH:11]=[C:12]([CH:19]=[CH:20][CH:21]=1)[C:13]([O:15][CH2:16][CH2:17][O:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)=[O:14])=[O:8])(=[O:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 31236PhenoxyethanolHCID 15670238HCID 15670238、化合物

生成物 1

HCID 15670239HCID 15670239、化合物収率 51.9%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 8471Triethylamine溶媒

反応条件

温度
60 °C

実験手順

Cyanomethyl 3-[(2 acetylthiomethyl-3-phenylpropionyl)amino]benzoate (compound of Example 116) (4 g), 2-phenoxyethanol (3 g), 4-dimethylaminopyridine (0.1 g) and triethylamine (2 g) are mixed, and the mixture is stirred at 60° C. for 15 hours and extracted with ethyl acetate (50 ml). The extract is washed with 10% hydrochloric acid and water, and ethyl acetate is distilled off under reduced pressure. The residue is dissolved in 50% aqueous acetonitrile and purified by a column chromatography using Diaion HP-20 (eluant, water-acetonitrile). The fractions containing the desired compound are collected, and acetonitrile is distilled off under reduced pressure. The aqueous solution is extracted with ethyl acetate (100 ml). The extract is dried over anhydrous magnesium sulfate, and ethyl acetate is distilled off under reduced pressure to give the title compound (2.5 g).

後処理

  1. extractionextracted with ethyl acetate (50 ml)
  2. washThe extract is washed with 10% hydrochloric acid and water, and ethyl acetate
  3. distillationis distilled off under reduced pressure
  4. dissolutionThe residue is dissolved in 50% aqueous acetonitrile
  5. custompurified by a column chromatography
  6. additionThe fractions containing the desired compound
  7. customare collected
  8. distillationacetonitrile is distilled off under reduced pressure
  9. extractionThe aqueous solution is extracted with ethyl acetate (100 ml)
  10. dry with materialThe extract is dried over anhydrous magnesium sulfate, and ethyl acetate
  11. distillationis distilled off under reduced pressure

出典と根拠

ORDレコード
ord-a9bfba8f528c4d658a91749fd406923a
出典データセット
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05210266

反応ノート

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