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2-Chloroacetophenone → N-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-4-phenyl-2-thiazolamine

HRID 2106747
ノート
印刷プレビュー

反応式

HRID 2106747 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12]([C:15]3[CH:20]=[CH:19][C:18]([NH:21][C:22]([NH2:24])=[S:23])=[CH:17][CH:16]=3)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1.Cl[CH2:26][C:27]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)=O.C([O-])(=O)C.[Na+]>C(O)(=O)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12]([C:15]3[CH:20]=[CH:19][C:18]([NH:21][C:22]4[S:23][CH:26]=[C:27]([C:29]5[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=5)[N:24]=4)=[CH:17][CH:16]=3)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1
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

5

反応物 3

HCID 107572-ChloroacetophenoneHCID 517045Sodium AcetateHCID 15125461N-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]thiourea

生成物 1

HCID 15125462N-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-4-phenyl-2-thiazolamine収率 69.6%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
80 °C

実験手順

A mixture of 5 parts of N-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]thiourea, 3 parts of 2-chloro-1-phenylethanone, 1.7 parts of sodium acetate and 100 parts of acetic acid was stirred for 4 hours at 80° C. After cooling, the reaction mixture was evaporated and the residue was stirred in 130 parts of dichloromethane. The whole was neutralised with a sodium hydrogen carbonate solution. The precipitated product was filtered off, washed with water and dichloromethane and crystallized from 1,4-dioxane. The product was filtered off and dried, yielding 4.5 parts (69.6%) of N-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-4-phenyl-2-thiazolamine; mp. 269.7° C. (int. 2).

後処理

  1. temperatureAfter cooling
  2. customthe reaction mixture was evaporated
  3. stirringthe residue was stirred in 130 parts of dichloromethane
  4. filtrationThe precipitated product was filtered off
  5. washwashed with water and dichloromethane
  6. customcrystallized from 1,4-dioxane
  7. filtrationThe product was filtered off
  8. customdried

出典と根拠

ORDレコード
ord-c6a228a124e34143a15f46e28a121744
出典データセット
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04931444

反応ノート

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