Potassium Carbonate → Methyl 4-[1-(benzenesulphonyl)-piperazin-4-ylmethyl]-benzoate

HRID 2290451

反応式

HRID 2290451 の反応式
Br[CH2:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][CH:4]=1.[C:13]1([S:19]([N:22]2[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]2)(=[O:21])=[O:20])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+]>CC(=O)CC>[C:13]1([S:19]([N:22]2[CH2:27][CH2:26][N:25]([CH2:2][C:3]3[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][CH:4]=3)[CH2:24][CH2:23]2)(=[O:21])=[O:20])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 256687Methyl 4-(bromomethyl)benzoateHCID 8087121-(Benzenesulfonyl)piperazine

生成物 1

HCID 8743532Methyl 4-[1-(benzenesulphonyl)-piperazin-4-ylmethyl]-benzoate

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

A mixture of 11.5 g. (50 mmole) methyl 4-bromomethylbenzoate, 11.3 g. (50 mmole) 1-benzenesulphonylpiperazine, 6.91 g. (50 mmole) powdered potassium carbonate and 100 ml. butan-2-one is maintained at reflux temperature for 20 hours, then suction filtered while hot and the filtrate evaporated. After cooling, the product is filtered off with suction and recrystallised from methanol to give 11.6 g. (62% of theory) of the desired product; m.p. 145°-146° C.

後処理

  1. additionA mixture of 11.5 g
  2. temperatureat reflux temperature for 20 hours
  3. filtrationsuction filtered while hot and the filtrate
  4. customevaporated
  5. temperatureAfter cooling
  6. filtrationthe product is filtered off with suction
  7. customrecrystallised from methanol
  8. customto give 11.6 g

出典と根拠

ORDレコード
ord-3b0bc9d052a841da8602a09a7a0a9eea
出典データセット
uspto-grants-1986_10
特許番号
US04616086

関連ノート

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