Hydrazine hydrate (1:1) → 2-(3-{[5-(4-Methoxyphenyl)-6-phenylfuro[2,3-d]pyrimidin-4-yl]amino}phenyl)acetic hydrazide

HRID 2189033ノート

反応式

HRID 2189033 の反応式
O.[NH2:2][NH2:3].CO[C:6](=[O:38])[CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([NH:14][C:15]2[C:16]3[C:23]([C:24]4[CH:29]=[CH:28][C:27]([O:30][CH3:31])=[CH:26][CH:25]=4)=[C:22]([C:32]4[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=4)[O:21][C:17]=3[N:18]=[CH:19][N:20]=2)[CH:9]=1>C1COCC1.CO>[CH3:31][O:30][C:27]1[CH:28]=[CH:29][C:24]([C:23]2[C:16]3[C:15]([NH:14][C:10]4[CH:9]=[C:8]([CH2:7][C:6]([NH:2][NH2:3])=[O:38])[CH:13]=[CH:12][CH:11]=4)=[N:20][CH:19]=[N:18][C:17]=3[O:21][C:22]=2[C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)=[CH:25][CH:26]=1

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 250953893-{[5-(4-Methoxy-phenyl)-6-phenylfuro[2,3-d]pyrimidin-4-yl]amino}phenylacetic acid methyl ester

生成物 1

HCID 582802042-(3-{[5-(4-Methoxyphenyl)-6-phenylfuro[2,3-d]pyrimidin-4-yl]amino}phenyl)acetic hydrazide

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
65 °C

実験手順

Add 215 mg (4.3 mmol) of hydrazine hydrate at RT to 100 mg (0.215 mmol) of 3-{[5-(4-methoxy-phenyl)-6-phenylfuro[2,3-d]pyrimidin-4-yl]amino}phenylacetic acid methyl ester (Example 28), dissolved in 1.5 ml of THF and 2 ml of methanol. Stir the mixture at 65° C. for 1 h and at RT overnight and then concentrate under reduced pressure. After stirring with diisopropyl ether, filter off the solid with suction and dry under reduced pressure. 89.3 mg (89.3% of theory) of the target product are obtained.

後処理

  1. concentrationat RT overnight and then concentrate under reduced pressure
  2. stirringAfter stirring with diisopropyl ether
  3. filtrationfilter off the solid with suction
  4. customdry under reduced pressure
  5. custom89.3 mg (89.3% of theory) of the target product are obtained

出典と根拠

ORDレコード
ord-8d0423d0fb90403f996cad11d2b17268
出典データセット
uspto-grants-2012_12
特許番号
US08324222B2

反応ノート

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