Ethyl chloroformate → HCID 22745278、化合物

HRID 47536ノート

反応式

HRID 47536 の反応式
[NH:1]1[CH2:6][CH2:5][CH:4]([N:7]2[CH2:12][CH2:11][CH:10]([N:13]3[C:17]4[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=4[NH:15][C:14]3=[O:22])[CH2:9][CH2:8]2)[CH2:3][CH2:2]1.C(N(C(C)C)CC)(C)C.Cl[C:33]([O:35][CH2:36][CH3:37])=[O:34].C(=O)(O)[O-].[Na+]>ClCCl.C(Cl)(Cl)Cl>[CH2:36]([O:35][C:33]([N:1]1[CH2:2][CH2:3][CH:4]([N:7]2[CH2:8][CH2:9][CH:10]([N:13]3[C:17]4[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=4[NH:15][C:14]3=[O:22])[CH2:11][CH2:12]2)[CH2:5][CH2:6]1)=[O:34])[CH3:37]

参加物

7

反応物 4

HCID 10928Ethyl chloroformateHCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 158395521-[1-(piperidin-4-yl)piperidin-4-yl]-1,3-dihydro-2H-benzimidazol-2-one

生成物 1

HCID 22745278HCID 22745278、化合物

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒

実験手順

Forty-one (41) mg of 1-[1-(piperidin-4-yl)piperidin-4-yl]-1,3-dihydro-2H-benzimidazol-2-one.di-trifluoroacetate was dissolved in 5 ml of dichloromethane, and to which 25 mg of diisopropylethylamine and 11 mg of ethyl chloroformate were added, followed by stirring overnight. The reaction mixture was distributed between chloroform and saturated aqueous sodium bicarbonate solution. The organic layer was dried over sodium sulfate, concentrated, and the resulting residue was purified by silica gel column chromatography (chloroform/methanol=10/1). Thus 22 mg of the title compound was obtained as a colorless, amorphous substance.

後処理

  1. dry with materialThe organic layer was dried over sodium sulfate
  2. concentrationconcentrated
  3. customthe resulting residue was purified by silica gel column chromatography (chloroform/methanol=10/1)

出典と根拠

ORDレコード
ord-6937df9d37f548408df6e1ac1e544ea5
出典データセット
uspto-grants-2004_03
特許番号
US06699880B1

反応ノート

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