Benzyl 1-(2-(4-(4-acetylpiperazin-1-yl)phenylamino)-5-fluoropyrimidin-4-yl)piperidin-4-ylcarbamate → 1-(4-(4-(4-(4-Aminopiperidin-1-yl)-5-fluoropyrimidin-2-ylamino)phenyl)piperazin-1-yl)ethanone

HRID 2281534ノート

反応式

HRID 2281534 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[CH:15]=[CH:14][C:13]([NH:16][C:17]3[N:22]=[C:21]([N:23]4[CH2:28][CH2:27][CH:26]([NH:29]C(=O)OCC5C=CC=CC=5)[CH2:25][CH2:24]4)[C:20]([F:40])=[CH:19][N:18]=3)=[CH:12][CH:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[H][H]>CO.[Pd]>[NH2:29][CH:26]1[CH2:27][CH2:28][N:23]([C:21]2[C:20]([F:40])=[CH:19][N:18]=[C:17]([NH:16][C:13]3[CH:12]=[CH:11][C:10]([N:7]4[CH2:8][CH2:9][N:4]([C:1](=[O:3])[CH3:2])[CH2:5][CH2:6]4)=[CH:15][CH:14]=3)[N:22]=2)[CH2:24][CH2:25]1

参加物

5

反応物 2

HCID 44467167Benzyl 1-(2-(4-(4-acetylpiperazin-1-yl)phenylamino)-5-fluoropyrimidin-4-yl)piperidin-4-ylcarbamateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 444671681-(4-(4-(4-(4-Aminopiperidin-1-yl)-5-fluoropyrimidin-2-ylamino)phenyl)piperazin-1-yl)ethanone収率 85.5%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A solution of benzyl 1-(2-(4-(4-acetylpiperazin-1-yl)phenylamino)-5-fluoropyrimidin-4-yl)piperidin-4-ylcarbamate (370 mg, 0.676 mmol) and Pd—C (10%, 55 mg) in MeOH (12 mL) was hydrogenated under balloon hydrogen for 20 h. It was then filtered through celite. The filtrate was concentrated in vacuo to give the titled compound (239 mg). MS 414.3 (M+H); UV 202.8, 268.8 nm.

後処理

  1. filtrationIt was then filtered through celite
  2. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-1beba1b248f94f2f89a5b7048bad0672
出典データセット
uspto-grants-2015_09
特許番号
US09139581B2

反応ノート

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