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Chloroacetyl chloride → 1,1-Dimethylethyl 4-(chloroacetyl)-3-[hydroxy(diphenyl)methyl]piperazine-1-carboxylate

HRID 1713505
ノート
印刷プレビュー

反応式

HRID 1713505 の反応式
[OH:1][C:2]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[CH:3]1[NH:8][CH2:7][CH2:6][N:5]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:4]1.C(N(C(C)C)CC)(C)C.[Cl:37][CH2:38][C:39](Cl)=[O:40].C(OCC)(=O)C>O1CCCC1>[Cl:37][CH2:38][C:39]([N:8]1[CH2:7][CH2:6][N:5]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:4][CH:3]1[C:2]([OH:1])([C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:40]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6577Chloroacetyl chlorideHCID 8857Ethyl AcetateHCID 81531DiisopropylethylamineHCID 23122074(1,1-Dimethylethyl)3-(hydroxydiphenylmethyl)-1-piperazine carboxylate

生成物 1

HCID 684196211,1-Dimethylethyl 4-(chloroacetyl)-3-[hydroxy(diphenyl)methyl]piperazine-1-carboxylate収率 46%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

To a solution of 1,1-dimethylethyl 3-[hydroxy(diphenyl)methyl]-1-piperazine carboxylate (0.50 g, 1.4 mmol) in tetrahydrofuran (5 mL) were sequentially added diisopropylethylamine (2 mL) and chloroacetyl chloride (0.46 g, 4.1 mmol) with ice cooling, and the mixture was stirred for 4 hours while elevating the temperature to room temperature. To the reaction solution was added ethyl acetate, and the resulting mixture was washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified with silica gel column chromatography (hexane:ethyl acetate=4:1) to obtain the title compound (0.28 g, yield 46%).

後処理

  1. customto room temperature
  2. washthe resulting mixture was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified with silica gel column chromatography (hexane:ethyl acetate=4:1)

出典と根拠

ORDレコード
ord-c38e1ae7b0d04d508f5b9bdb775befe9
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07795267B2

反応ノート

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