Trifluoroacetic acid → HCID 67215444、化合物

HRID 472904ノート

反応式

HRID 472904 の反応式
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]

参加物

5

反応物 2

HCID 6422Trifluoroacetic acidHCID 67216035HCID 67216035、化合物

生成物 1

HCID 67215444HCID 67215444、化合物収率 85.2%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 6344Dichloromethane溶媒

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-9ebfd19d5c144a09b379c07b0c2c384d
出典データセット
uspto-grants-2014_01
特許番号
US08633216B2

反応ノート

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