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Sodium Carbonate → HCID 131716287、化合物

HRID 1084756
ノート
印刷プレビュー

反応式

HRID 1084756 の反応式
Br[CH2:2][CH2:3][N:4]1[C:8](=[O:9])[N:7]([CH2:10][CH3:11])[N:6]=[N:5]1.[CH3:12][C:13]1[O:17][C:16]([CH2:18][N:19]2[C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[N:21]=[C:20]2[NH:28][CH:29]2[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]2)=[CH:15][CH:14]=1.[C:35](=[O:38])([O-:37])[O-].[Na+].[Na+].CN(C)C(=O)C>O>[C:8]([OH:9])(=[O:17])[C:35]([OH:37])=[O:38].[CH2:10]([N:7]1[C:8](=[O:9])[N:4]([CH2:3][CH2:2][N:32]2[CH2:33][CH2:34][CH:29]([NH:28][C:20]3[N:19]([CH2:18][C:16]4[O:17][C:13]([CH3:12])=[CH:14][CH:15]=4)[C:23]4[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=4[N:21]=3)[CH2:30][CH2:31]2)[N:5]=[N:6]1)[CH3:11]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 10340Sodium CarbonateHCID 31374DimethylacetamideHCID 30199151-(2-Bromoethyl)-4-ethyl-1,4-dihydro-5H-tetrazol-5-oneHCID 14677561HCID 14677561、化合物

生成物 1

HCID 131716287HCID 131716287、化合物収率 55%

試薬・触媒・溶媒 1

HCID 962Water
溶媒

反応条件

温度
80 °C

実験手順

A mixture of 3.32 parts of 1-(2-bromoethyl)-4-ethyl-1,4-dihydro-5H-tetrazol-5-one, 4.65 parts of 1-[(5-methyl-2-furanyl)methyl]-N-(4-piperidinyl)-1H-benzimidazol-2-amine, 1.6 parts of sodium carbonate and 45 parts of N,N-dimethylacetamide was stirred overnight at 80° C. The reaction mixture was poured into water and the product was extracted with 4-methyl-2-pentanone. The extract was dried, filtered and evaporated. The residue was purified by filtration over silica gel using a mixture of trichloromethane and methanol (96:4 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was converted into the ethanedioate salt in methanol. The salt was filtered off and dried, yielding 5.2 parts (55%) of 1-ethyl-1,4-dihydro-4-[2-[4-[[1-[(5-methyl-2-furanyl)methyl]-1H-benzimidazol-2-yl]-amino]-1-piperidinyl]ethyl]-5H-tetrazol-5-one ethanedioate(1:2); mp. 190.5° C. (compound 22).

後処理

  1. extractionthe product was extracted with 4-methyl-2-pentanone
  2. customThe extract was dried
  3. filtrationfiltered
  4. customevaporated
  5. filtrationThe residue was purified by filtration over silica gel using
  6. additiona mixture of trichloromethane and methanol (96:4 by volume) as eluent
  7. customThe pure fractions were collected
  8. customthe eluent was evaporated
  9. filtrationThe salt was filtered off
  10. customdried

出典と根拠

ORDレコード
ord-b581ff6776b84f3f831957344f1e4d24
出典データセット
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05006527

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート