反応式
[F:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([N:8]2[CH2:10][CH2:9]2)=[O:7])=[CH:4][CH:3]=1.Cl.[O:14]=[C:15]1[N:19]([CH2:20][CH2:21][C:22]#[N:23])[C:18]2[CH:24]=[CH:25][CH:26]=[CH:27][C:17]=2[N:16]1[CH:28]1[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1.C(N(CC)CC)C.C1C=CC=CC=1>CO>[C:22]([CH2:21][CH2:20][N:19]1[C:18]2[CH:24]=[CH:25][CH:26]=[CH:27][C:17]=2[N:16]([CH:28]2[CH2:33][CH2:32][N:31]([CH2:9][CH2:10][NH:8][C:6](=[O:7])[C:5]3[CH:4]=[CH:3][C:2]([F:1])=[CH:12][CH:11]=3)[CH2:30][CH2:29]2)[C:15]1=[O:14])#[N:23]参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
A mixture of 1.68 parts of 1-(4-fluorobenzoyl)aziridine, 3.07 parts of 2,3-dihydro-2-oxo-3-(4-piperidinyl)-1H-benzimidazole-1-propanenitrile hydrochloride, 1.65 parts of N,N-diethylethanamine, 10.8 parts of benzene and 1.6 parts of methanol is stirred and refluxed for 1.50 hours. The reaction mixture is cooled and poured onto water. The product is extracted with trichloromethane. The extract is dried, filtered and evaporated. The residue is crystallized from 2-propanol. The product is filtered off and recrystallized from 2-propanol, yielding 1part of N-[2-{4-[3-(2-cyanoethyl)-2,3-dihydro-2-oxo-1H-benzimidazol-1-yl]-1-piperidinyl}ethyl]-4-fluorobenzamide; mp. 172.2° C.
後処理
- temperaturerefluxed for 1.50 hours
- temperatureThe reaction mixture is cooled
- additionpoured onto water
- extractionThe product is extracted with trichloromethane
- customThe extract is dried
- filtrationfiltered
- customevaporated
- customThe residue is crystallized from 2-propanol
- filtrationThe product is filtered off
- customrecrystallized from 2-propanol
出典と根拠
- ORDレコード
- ord-d430f8b65d8c48dfbff9d02feace18b1
- 出典データセット
- uspto-grants-1977_06
- 特許番号
- US04031226
関連ノート
読み込み中…