Methylamine → N-(4-{2-[6-(4-chlorophenyl)-4-oxothieno[3,2-d]pyrimidin-3(4H)-yl]ethyl}benzyl)-N,N2-dimethylglycinamide

HRID 1668402노트

반응식

HRID 1668402 반응식
Cl[CH2:2][C:3]([N:5]([CH2:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][N:16]2[C:21](=[O:22])[C:20]3[S:23][C:24]([C:26]4[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][CH:27]=4)=[CH:25][C:19]=3[N:18]=[CH:17]2)=[CH:10][CH:9]=1)[CH3:6])=[O:4].[CH3:33][NH2:34]>CO.CN(C)C=O.C(OCC)(=O)C>[Cl:32][C:29]1[CH:30]=[CH:31][C:26]([C:24]2[S:23][C:20]3[C:21](=[O:22])[N:16]([CH2:15][CH2:14][C:11]4[CH:12]=[CH:13][C:8]([CH2:7][N:5]([CH3:6])[C:3](=[O:4])[CH2:2][NH:34][CH3:33])=[CH:9][CH:10]=4)[CH:17]=[N:18][C:19]=3[CH:25]=2)=[CH:27][CH:28]=1

참가 물질

6

반응물 2

HCID 6329MethylamineHCID 592398302-chloro-N-(4-{2-[6-(4-chlorophenyl)-4-oxothieno[3,2-d]pyrimidin-3(4H)-yl]ethyl}benzyl)-N-methylacetamide

생성물 1

HCID 59239845N-(4-{2-[6-(4-chlorophenyl)-4-oxothieno[3,2-d]pyrimidin-3(4H)-yl]ethyl}benzyl)-N,N2-dimethylglycinamide

시약·촉매·용매 3

HCID 887Methanol용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of the compound (0.12 g) obtained in Example 27, 40% methylamine in methanol solution (0.28 ml) and N,N-dimethylformamide (2 ml) was stirred at room temperature for 1 hr, diluted with ethyl acetate, washed with water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate-hexane (1:1, volume ratio) to give the title compound (53 mg) as a colorless powder.

후처리

  1. washwashed with water and saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was recrystallized from ethyl acetate-hexane (1:1, volume ratio)

출처 및 근거

ORD 기록
ord-bc8166d171034202b405a64e4d4dbd83
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07989445B2

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