Sodium Carbonate → HCID 178433270、化合物

HRID 979928ノート

反応式

HRID 979928 の反応式
Cl.Cl[CH2:3][C:4]1[NH:8][CH:7]=[N:6][C:5]=1[CH3:9].[O:10]1[CH:14]=[CH:13][CH:12]=[C:11]1[CH2:15][N:16]1[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[N:18]=[C:17]1[NH:25][CH:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1.C(=O)([O-])[O-].[Na+].[Na+]>CN(C)C=O>[O:10]1[CH:14]=[CH:13][CH:12]=[C:11]1[CH2:15][N:16]1[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[N:18]=[C:17]1[NH:25][CH:26]1[CH2:27][CH2:28][N:29]([CH2:3][C:4]2[NH:8][CH:7]=[N:6][C:5]=2[CH3:9])[CH2:30][CH2:31]1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 135879951-(2-furanylmethyl)-N-(4-piperidinyl)-1H-benzimidazol-2-amineHCID 178433265HCID 178433265、化合物

生成物 1

HCID 178433270HCID 178433270、化合物収率 60.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

A mixture of 3.4 parts of 5-(chloromethyl)-4-methyl-1H-imidazole monohydrochloride, 6 parts of 1-(2-furanylmethyl)-N-(4-piperidinyl)-1H-benzimidazol-2-amine, 4.25 parts of sodium carbonate and 135 parts of N,N-dimethylformamide was stirred and heated for 3 hours at 70° C. The reaction mixture was poured onto water and the product was extracted with trichloromethane. The extract was dried, filtered and evaporated. The residue was crystallized from a mixture of acetonitrile and methanol, yielding 4.7 parts (60.2%) of 1-(2-furanylmethyl)-N-[1-[(4-methyl-1H-imidazol-5-yl)methyl]-4-piperidinyl]-1H-benzimidazol-2-amine; mp. 242.1° C. (compound 1).

後処理

  1. additionThe reaction mixture was poured onto water
  2. extractionthe product was extracted with trichloromethane
  3. customThe extract was dried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was crystallized from a mixture of acetonitrile and methanol

出典と根拠

ORDレコード
ord-2a73bbde20974649b7506ceaa3b5686c
出典データセット
uspto-grants-1987_01
特許番号
US04634704

反応ノート

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