Tetrahydrofuran → 2-(5-Amino-2-ethoxyphenyl)-5-methyl-7-cyclopentyl-3H-imidazo[5,1-f][1,2,4]-triazin-4-one

HRID 11265

反応式

O1CCCC1.[CH2:6]([O:8][C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-])=O)=[CH:11][C:10]=1[C:18]1[NH:23][C:22](=[O:24])[C:21]2=[C:25]([CH3:33])[N:26]=[C:27]([CH:28]3[CH2:32][CH2:31][CH2:30][CH2:29]3)[N:20]2[N:19]=1)[CH3:7]>C(O)C.[Pd]>[NH2:15][C:12]1[CH:13]=[CH:14][C:9]([O:8][CH2:6][CH3:7])=[C:10]([C:18]2[NH:23][C:22](=[O:24])[C:21]3=[C:25]([CH3:33])[N:26]=[C:27]([CH:28]4[CH2:32][CH2:31][CH2:30][CH2:29]4)[N:20]3[N:19]=2)[CH:11]=1

参加物

実験手順

In 86 ml of ethanol and 86 ml of tetrahydrofuran 2.56 g (6.68 mmol) of the compound from example 41A are stirred in the presence of 288 mg of Pd/C (10%) under an H2 atmosphere for 20 hours. The reaction solution is filtered with suction through 30 ml of silica gel, the filter cake is washed with ethanol/tetrahydrofuran and the filtrate is concentrated and dried under high vacuum overnight. The crude product is chromatographed on 500 ml of silica gel using toluene and ethyl acetate in a gradient system.

後処理

filtrationThe reaction solution is filtered with suction through 30 ml of silica gel
washthe filter cake is washed with ethanol/tetrahydrofuran
concentrationthe filtrate is concentrated
customdried under high vacuum overnight
customThe crude product is chromatographed on 500 ml of silica gel

出典と根拠

ORDレコード: ord-d357c1218dbf48bba5a042e2f55bdc08
出典データセット: uspto-grants-2006_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07098207B2

反応式

参加物

反応物 2

生成物 1

試薬・触媒・溶媒 2

実験手順

後処理

出典と根拠

関連ノート