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Triethylamine → HCID 68643979、化合物

HRID 2388702
ノート
印刷プレビュー

反応式

HRID 2388702 の反応式
[C:1]1([CH:7]2[CH:12]=[C:11]([N:13]3[CH2:17][CH2:16][CH2:15][CH2:14]3)[CH2:10][CH2:9][N:8]2[C:18](=[O:20])[CH3:19])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:22](=[N:28][OH:29])[C:23]([O:25][CH2:26][CH3:27])=[O:24].C(N(CC)CC)C>ClCCl>[C:18]([N:8]1[CH2:9][CH2:10][C:11]2([N:13]3[CH2:14][CH2:15][CH2:16][CH2:17]3)[O:29][N:28]=[C:22]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:12]2[CH:7]1[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)(=[O:20])[CH3:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 6816376Ethyl chloro(hydroximino)acetateHCID 68643976HCID 68643976、化合物

生成物 1

HCID 68643979HCID 68643979、化合物収率 80%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 1-(2-phenyl-4-(pyrrolidin-1-yl)-5,6-dihydropyridin-1(2H)-yl)ethanone in dichloromethane (15 mL) was added a solution of ethyl 2-chloro-2-(hydroxyimino)acetate (4.709 mmol, 1.4 eq.) in dichloromethane (5 ml) at 0° C. Then triethylamine (1.4 eq.) was added dropwise at same reaction conditions and the mixture was stirred at room temperature overnight. The reaction mixture was quenched with 10% citric acid solution and extracted with dichloromethane (3×). The combined organic layers were washed with saturated sodium bicarbonate solution and brine, dried over sodium sulfate, concentrated to dryness to give the desired product, which was used in the next step without further purification.

後処理

  1. customThe reaction mixture was quenched with 10% citric acid solution
  2. extractionextracted with dichloromethane (3×)
  3. washThe combined organic layers were washed with saturated sodium bicarbonate solution and brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-7cb4966bdba4478da42e06ca95fd7622
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08268814B2

反応ノート

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