Isobutyraldehyde → HCID 16048759、化合物

HRID 1364146ノート

反応式

HRID 1364146 の反応式
[N:1]1[N:2]([C:11]2[CH:19]=[CH:18][C:14]([C:15]([NH2:17])=[O:16])=[CH:13][CH:12]=2)[CH:3]=[C:4]2[CH2:10][CH2:9][NH:8][CH2:7][CH2:6][C:5]=12.[CH3:20][CH:21]([CH3:24])[CH:22]=O.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCl.C(O)(=O)C.CO>[CH3:20][CH:21]([CH3:24])[CH2:22][N:8]1[CH2:9][CH2:10][C:4]2=[CH:3][N:2]([C:11]3[CH:19]=[CH:18][C:14]([C:15]([NH2:17])=[O:16])=[CH:13][CH:12]=3)[N:1]=[C:5]2[CH2:6][CH2:7]1

参加物

7

反応物 3

HCID 6561IsobutyraldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 66930841HCID 66930841、化合物

生成物 1

HCID 16048759HCID 16048759、化合物

試薬・触媒・溶媒 3

HCID 176Acetic Acid触媒HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-(5,6,7,8-tetrahydropyrazolo[3,4-d]azepin-2(4H)-yl)benzamide (may be prepared as described in Description 37) (31 mg, 0.12 mmol) in dichloromethane (3 ml) was added 2-methylpropanal (17 mg, 0.24 mmol) and acetic acid (2 drops). The resulting mixture was stirred at room temperature, under argon, for 20 minutes. Sodium triacetoxyborohydride (51 mg, 0.24 mmol) was added and stirring continued for 2 hours. The resulting crude mixture was diluted with methanol and then purified by SCX, eluting with methanol and then with 2M ammonia/methanol. The basic fractions were combined and solvent evaporated in vacuo to afford the title compound (E16). MS (ES+) m/e 313 [M+H]+.

後処理

  1. stirringstirring
  2. waitcontinued for 2 hours
  3. custompurified by SCX
  4. washeluting with methanol
  5. customsolvent evaporated in vacuo

出典と根拠

ORDレコード
ord-c544ea5f42534d82bd5f4e10c717be40
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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