Triethylamine → N-(2,6-dimethylphenyl)hexahydro-3,3-dimethyl-2-(1-methylethyl)-1-oxoimidazo[1,5-a]pyrazine-7(8H)-acetamide

HRID 35332

反応式

HRID 35332 の反応式
Cl[CH2:2][C:3]([NH:5][C:6]1[C:11]([CH3:12])=[CH:10][CH:9]=[CH:8][C:7]=1[CH3:13])=[O:4].[CH3:14][C:15]1([CH3:28])[N:19]2[CH2:20][CH2:21][NH:22][CH2:23][CH:18]2[C:17](=[O:24])[N:16]1[CH:25]([CH3:27])[CH3:26].C(N(CC)CC)C>CN(C)C=O>[CH3:13][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]([CH3:12])[C:6]=1[NH:5][C:3](=[O:4])[CH2:2][N:22]1[CH2:21][CH2:20][N:19]2[C:15]([CH3:14])([CH3:28])[N:16]([CH:25]([CH3:26])[CH3:27])[C:17](=[O:24])[CH:18]2[CH2:23]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 707982-Chloro-N-(2,6-dimethylphenyl)acetamideHCID 21295654hexahydro-3,3-dimethyl-2-(1-methylethyl)imidazo[1,5-a]pyrazin-1(5H)-one

生成物 1

HCID 14230242N-(2,6-dimethylphenyl)hexahydro-3,3-dimethyl-2-(1-methylethyl)-1-oxoimidazo[1,5-a]pyrazine-7(8H)-acetamide収率 72.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
75 °C

実験手順

A mixture of 8.2 parts of 2-chloro-N-(2,6-dimethylphenyl)acetamide, 7.2 parts of hexahydro-3,3-dimethyl-2-(1-methylethyl)imidazo[1,5-a]pyrazin-1(5H)-one, 7 parts of N,N-diethylethanamine and 54 parts of N,N-dimethylformamide was stirred and heated for 3 hours at 75° C. After cooling to 0° C., the precipitate was filtered off and the filtrate was evaporated. The residue was dissolved in 300 parts of trichloromethane. This solution was washed with 50 parts of water, dried, filtered and evaporated. The residue was triturated in 2,2'-oxybispropane. After cooling to 0° C., the product was filtered off and dried, yielding 9.2 parts (72.7%) of N-(2,6-dimethylphenyl)hexahydro-3,3-dimethyl-2-(1-methylethyl)-1-oxoimidazo[1,5-a]pyrazine-7(8H)-acetamide; mp. 155° C. (intermediate 101).

後処理

  1. temperatureAfter cooling to 0° C.
  2. filtrationthe precipitate was filtered off
  3. customthe filtrate was evaporated
  4. dissolutionThe residue was dissolved in 300 parts of trichloromethane
  5. washThis solution was washed with 50 parts of water
  6. customdried
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue was triturated in 2,2'-oxybispropane
  10. temperatureAfter cooling to 0° C.
  11. filtrationthe product was filtered off
  12. customdried

出典と根拠

ORDレコード
ord-aefb654b87b7431f99ffecb3fefb8341
出典データセット
uspto-grants-1988_08
特許番号
US04766125

関連ノート

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