Ethyl chloroformate → HCID 22745278, 화합물

HRID 47536노트

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HRID 47536 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 22745278HCID 22745278, 화합물

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-6937df9d37f548408df6e1ac1e544ea5
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699880B1

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