Isobutyraldehyde → HCID 16048759, 화합물

HRID 1364146노트

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HRID 1364146 반응식
[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

참가 물질

7

반응물 3

HCID 6561IsobutyraldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 66930841HCID 66930841, 화합물

생성물 1

HCID 16048759HCID 16048759, 화합물

시약·촉매·용매 3

HCID 176Acetic Acid촉매HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

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]+.

후처리

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

출처 및 근거

ORD 기록
ord-c544ea5f42534d82bd5f4e10c717be40
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07888347B2

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