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Dimethylformamide → HCID 13344910, 화합물

HRID 2164817
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HRID 2164817 반응식
[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[NH:13][C:14]([N:16]1[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]1)=S.CN(C)C=O.[C:28](=[O:31])([O-:30])[O-].[K+].[K+].N#CBr.[C:37]([O:40]CC)(=[O:39])[CH3:38]>CCOCC>[C:37]([OH:40])(=[O:39])/[CH:38]=[CH:2]\[C:28]([OH:30])=[O:31].[CH3:22][N:19]1[CH2:20][CH2:21][N:16]([C:14]2[N:3]3[CH:4]=[CH:5][N:1]=[C:2]3[CH2:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[N:13]=2)[CH2:17][CH2:18]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 6228DimethylformamideHCID 8857Ethyl AcetateHCID 10476Cyanogen BromideHCID 11430Potassium CarbonateHCID 204033081-[2-(2-Imidazolylmethyl) phenylthiocarbamoyl]-4-methylpiperazine

생성물 1

HCID 13344910HCID 13344910, 화합물

시약·촉매·용매 1

HCID 3283
Diethyl Ether
용매

실험 절차

The mixture of 315 mg of 1-[2-(2-imidazolylmethyl)phenylthiocarbamoyl]-4-methylpiperazine, 3.3 ml of dimethylformamide, 276 mg of potassium carbonate, 116 mg of cyanogen bromide and 50 mg of 8-crown-6 ether is stirred at room temperature under nitrogen for 3 hours. It is diluted with ethyl acetate, washed with saturated aqueous sodium chloride, dried and evaporated. The residue is dissolved in acetone, the solution treated with 116 mg of maleic acid and diluted with diethyl ether, to yield 5-(4-methyl-1-piperazinyl)-11H-imidazo[1,2-c][1,3]benzodiazepine monomaleate of example 1.

후처리

  1. washwashed with saturated aqueous sodium chloride
  2. customdried
  3. customevaporated
  4. dissolutionThe residue is dissolved in acetone
  5. additionthe solution treated with 116 mg of maleic acid
  6. additiondiluted with diethyl ether

출처 및 근거

ORD 기록
ord-656aa81d79b34c16a903d02fb56d6c78
출처 데이터셋
uspto-grants-1985_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04507311

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