Trifluoroacetic acid → HCID 67215444, 화합물

HRID 472904노트

반응식

HRID 472904 반응식
FC(F)(F)C(O)=O.[CH3:8][O:9][C:10]([C:12]1[CH:13]=[C:14]([CH:33]=[CH:34][C:35]=1[N+:36]([O-:38])=[O:37])[C:15]([C:17]1[N:21]2[CH:22]=[C:23]([C:26]([O:28]C(C)(C)C)=[O:27])[CH:24]=[CH:25][C:20]2=[CH:19][N:18]=1)=[O:16])=[O:11]>ClCCl.CC(C)=O>[CH3:8][O:9][C:10]([C:12]1[CH:13]=[C:14]([CH:33]=[CH:34][C:35]=1[N+:36]([O-:38])=[O:37])[C:15]([C:17]1[N:21]2[CH:22]=[C:23]([C:26]([OH:28])=[O:27])[CH:24]=[CH:25][C:20]2=[CH:19][N:18]=1)=[O:16])=[O:11]

참가 물질

5

반응물 2

HCID 6422Trifluoroacetic acidHCID 67216035HCID 67216035, 화합물

생성물 1

HCID 67215444HCID 67215444, 화합물수율 85.2%

시약·촉매·용매 2

HCID 180Acetone용매HCID 6344Dichloromethane용매

실험 절차

2.13 ml (28.68 mmol) of trifluoroacetic acid are added to 610 mg (1.43 mmol) of tert-butyl 3-[3-(methoxycarbonyl)-4-nitrobenzoyl]imidazo[1,5-a]pyridine-6-carboxylate in 2 ml of dichloromethane and the mixture is stirred at ambient temperature for 5 hours. The reaction medium is concentrated under reduced pressure and then the residue obtained is taken up in acetone. The precipitate formed is filtered off, washed with acetone and dried. 450 mg of a yellow powder are obtained. Melting point: 290° C.; 1H NMR (d6-DMSO): 3.90 (3H, s), 7.78 (1H, d), 8.04 (1H, s), 8.12 (1H, d), 8.26 (1H, d), 8.68 (1H, d), 8.75 (1H, s), 10.26 (1H, s)

후처리

  1. concentrationThe reaction medium is concentrated under reduced pressure
  2. customthe residue obtained
  3. customThe precipitate formed
  4. filtrationis filtered off
  5. washwashed with acetone
  6. customdried

출처 및 근거

ORD 기록
ord-9ebfd19d5c144a09b379c07b0c2c384d
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08633216B2

반응 노트

불러오는 중…