Methylamine → 1,1-Dimethylethyl 2-{4-[(methylamino)carbonyl]phenyl}-4,5,7,8-tetrahydropyrazolo[3,4-d]azepine-6(2H)-carboxylate

HRID 1364119ノート

反応式

HRID 1364119 の反応式
[CH3:1][C:2]([O:5][C:6]([N:8]1[CH2:14][CH2:13][C:12]2=[CH:15][N:16]([C:18]3[CH:26]=[CH:25][C:21]([C:22]([OH:24])=O)=[CH:20][CH:19]=3)[N:17]=[C:11]2[CH2:10][CH2:9]1)=[O:7])([CH3:4])[CH3:3].O=[C:28](N1C=CN=C1)[N:29]1C=CN=C1.CN>ClCCl.O>[CH3:28][NH:29][C:22]([C:21]1[CH:20]=[CH:19][C:18]([N:16]2[CH:15]=[C:12]3[C:11]([CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:4])([CH3:3])[CH3:1])=[O:7])[CH2:14][CH2:13]3)=[N:17]2)=[CH:26][CH:25]=1)=[O:24]

参加物

6

反応物 3

HCID 6329MethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 669308134-[6-{[(1,1-dimethylethyl)oxy]carbonyl}-5,6,7,8-tetrahydropyrazolo[3,4-d]azepin-2(4H)-yl]benzoic acid

生成物 1

HCID 669307901,1-Dimethylethyl 2-{4-[(methylamino)carbonyl]phenyl}-4,5,7,8-tetrahydropyrazolo[3,4-d]azepine-6(2H)-carboxylate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a suspension of 4-[6-{[(1,1-dimethylethyl)oxy]carbonyl}-5,6,7,8-tetrahydropyrazolo[3,4-d]azepin-2(4H)-yl]benzoic acid (may be prepared as described in Description 23) (185 mg, 0.52 mmol) in dichloromethane (10 ml) was added 1,1′-(oxomethanediyl)bis-1H-imidazole (168 mg, 1.04 mmol) and the reaction stirred at room temperature, under argon, overnight. Methylamine (64 mg, 2.07 mmol) was added and stirring continued, under argon, at room temperature for 4 hours. The resulting crude mixture was diluted with water, and extracted with dichloromethane (×2). The combined organic fractions were washed with water (×1), dried over magnesium sulphate and solvent evaporated in vacuo to afford the title compound (D24). MS (ES+) m/e 371 [M+H]+.

後処理

  1. stirringstirring continued, under argon, at room temperature for 4 hours
  2. extractionextracted with dichloromethane (×2)
  3. washThe combined organic fractions were washed with water (×1)
  4. dry with materialdried over magnesium sulphate and solvent
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-7ff65d0791d54bc78091fbd4bf8f6c40
出典データセット
uspto-grants-2011_02
特許番号
US07888347B2

反応ノート

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