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

HRID 1668402ノート

反応式

HRID 1668402 の反応式
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

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-bc8166d171034202b405a64e4d4dbd83
出典データセット
uspto-grants-2011_08
特許番号
US07989445B2

反応ノート

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