Diisopropylethylamine → HCID 117666881、化合物

HRID 1526225ノート

反応式

HRID 1526225 の反応式
Cl[C:2]1[N:3]=[C:4]([NH:13][C:14]2[CH:19]=[CH:18][C:17]([N:20]3[CH2:25][CH2:24][CH:23]([N:26]4[CH2:31][CH2:30][N:29]([CH3:32])[CH2:28][CH2:27]4)[CH2:22][CH2:21]3)=[CH:16][CH:15]=2)[C:5]([C:10]([NH2:12])=[O:11])=[N:6][C:7]=1[CH2:8][CH3:9].[NH2:33][CH2:34][CH:35]1[CH2:40][CH2:39][N:38]([C:41]([O:43][C:44]([CH3:47])([CH3:46])[CH3:45])=[O:42])[CH2:37][CH2:36]1.C(N(C(C)C)CC)(C)C>CN1CCCC1=O>[C:10]([C:5]1[N:6]=[C:7]([CH2:8][CH3:9])[C:2]([NH:33][CH2:34][CH:35]2[CH2:40][CH2:39][N:38]([C:41]([O:43][C:44]([CH3:47])([CH3:46])[CH3:45])=[O:42])[CH2:37][CH2:36]2)=[N:3][C:4]=1[NH:13][C:14]1[CH:19]=[CH:18][C:17]([N:20]2[CH2:25][CH2:24][CH:23]([N:26]3[CH2:31][CH2:30][N:29]([CH3:32])[CH2:28][CH2:27]3)[CH2:22][CH2:21]2)=[CH:16][CH:15]=1)(=[O:11])[NH2:12]

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 7368171-Boc-4-(aminomethyl)piperidineHCID 885697085-Chloro-6-ethyl-3-({4-[4-(4-methylpiperazin-1-yl)piperidin-1-yl]phenyl}amino)pyrazine-2-carboxamide

生成物 1

HCID 117666881HCID 117666881、化合物

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

A mixture of 5-chloro-6-ethyl-3-({4-[4-(4-methylpiperazin-1-yl)piperidin-1-yl]phenyl}amino)pyrazine-2-carboxamide (200 mg), tert-butyl 4-(aminomethyl)piperidine-1-carboxylate (300 μL), diisopropylethylamine (240 μL), and N-methylpyrrolidone (0.8 mL) was reacted in a microwave reaction device at 160° C. for 2 hours. The mixture was subjected to liquid separation with ethyl acetate and water, and the organic phase was dried over magnesium sulfate, and then the solvent was evaporated under reduced pressure. The obtained residue was washed with diisopropyl ether to obtain tert-butyl 4-({[5-carbamoyl-3-ethyl-6-({4-[4-(4-methylpiperazin-1-yl)piperidin-1-yl]phenyl}amino)pyrazin-2-yl]amino}methyl)piperidine-1-carboxylate (195 mg) as a pale yellow solid.

後処理

  1. customwas reacted in a microwave reaction device at 160° C. for 2 hours
  2. customThe mixture was subjected to liquid separation with ethyl acetate and water
  3. dry with materialthe organic phase was dried over magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. washThe obtained residue was washed with diisopropyl ether

出典と根拠

ORDレコード
ord-75ece3596624462da1f881e24ca04679
出典データセット
uspto-grants-2015_07
特許番号
US09085540B2

反応ノート

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