Trifluoroacetic acid → {4-[1-Benzyl-6-(2-piperidin-4-yl-(E)-vinyl)-1H-indazol-3-yl]-piperidin-1-yl}-acetic acid trifluoroacetate
反応式
C(OC([N:8]1[CH2:13][CH2:12][CH:11](/[CH:14]=[CH:15]/[C:16]2[CH:24]=[C:23]3[C:19]([C:20]([CH:32]4[CH2:37][CH2:36][N:35]([CH2:38][C:39]([O:41]C(C)(C)C)=[O:40])[CH2:34][CH2:33]4)=[N:21][N:22]3[CH2:25][C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)=[CH:18][CH:17]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.[F:46][C:47]([F:52])([F:51])[C:48]([OH:50])=[O:49]>>[F:46][C:47]([F:52])([F:51])[C:48]([OH:50])=[O:49].[CH2:25]([N:22]1[C:23]2[C:19](=[CH:18][CH:17]=[C:16](/[CH:15]=[CH:14]/[CH:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)[CH:24]=2)[C:20]([CH:32]2[CH2:37][CH2:36][N:35]([CH2:38][C:39]([OH:41])=[O:40])[CH2:34][CH2:33]2)=[N:21]1)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1参加物
3
反応物 2
生成物 1
実験手順
4-{2-[1-Benzyl-3-(1-tert-butoxycarbonylmethyl-piperidin-4-yl]-1H-indazol-6-yl]-(E)-vinyl}-piperidine-1carboxylic acid tert-butyl ester (95 mg, 0.154 mmol) was treated with trifluoroacetic acid (2 ml) and the mixture stirred under nitrogen for 18 h. The solution was concentrated in vacuo and the residue dried in vacuo for 1 h. The resulting yellow gum was saturated with dry diethyl ether (5 ml); the supernatant was decanted off and the solid was washed with ether (5 ml) and dried in vacuo at 60° for 18 h to give the title compound (94 mg) as a pale yellow solid (94 mg).
後処理
- concentrationThe solution was concentrated in vacuo
- customthe residue dried in vacuo for 1 h
- customthe supernatant was decanted off
- washthe solid was washed with ether (5 ml)
- customdried in vacuo at 60° for 18 h
出典と根拠
- ORDレコード
- ord-dffcb20f5cc04208b48d4769647532f9
- 出典データセット
- uspto-grants-1999_01
- 特許番号
- US05861414
反応ノート
読み込み中…