Acetic Anhydride → HCID 12852070、化合物

HRID 1156360ノート

反応式

HRID 1156360 の反応式
[NH2:1][C:2]1[CH:27]=[CH:26][CH:25]=[CH:24][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][N:9]1[CH2:14][CH2:13][CH:12]([C:15](=[O:23])[C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)[CH2:11][CH2:10]1)=[O:5].[C:28](OC(=O)C)(=O)[CH3:29]>CC1C=CC=CC=1>[F:22][C:19]1[CH:18]=[CH:17][C:16]([C:15]([CH:12]2[CH2:11][CH2:10][N:9]([CH2:8][CH2:7][N:6]3[C:4](=[O:5])[C:3]4[C:2](=[CH:27][CH:26]=[CH:25][CH:24]=4)[N:1]=[C:28]3[CH3:29])[CH2:14][CH2:13]2)=[O:23])=[CH:21][CH:20]=1

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 30186512-Amino-N-{2-[4-(4-fluorobenzoyl)piperidin-1-yl]ethyl}benzene-1-carboximidic acid

生成物 1

HCID 12852070HCID 12852070、化合物収率 69%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 6 parts of 2-amino-N-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]benzamide, 10 parts of acetic acid anhydride and 108 parts of methylbenzene is stirred and refluxed overnight. The reaction mixture is evaporated and water is added to the oily residue. The whole is alkalized with a dilute sodium hydroxide solution and extracted with trichloromethane. The extract is dried, filtered and evaporated. The oily residue is crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane. The product is filtered off and recrystallized from 2-propanol, yielding 4.4 parts (69%) of 3-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]-2-methyl-4(3H)-quinazolinone; mp. 164.9° C.

後処理

  1. temperaturerefluxed overnight
  2. customThe reaction mixture is evaporated
  3. additionwater is added to the oily residue
  4. extractionextracted with trichloromethane
  5. customThe extract is dried
  6. filtrationfiltered
  7. customevaporated
  8. customThe oily residue is crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane
  9. filtrationThe product is filtered off
  10. customrecrystallized from 2-propanol

出典と根拠

ORDレコード
ord-2948e088ab744011aaca82c7c0f5233c
出典データセット
uspto-grants-1982_06
特許番号
US04335127

反応ノート

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