Piperazine Dihydrochloride → Methyl 4-[(piperazin-1-yl)methyl]benzoate

HRID 2290450

反応式

HRID 2290450 の反応式
O.O.O.O.O.O.[NH:7]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1.Cl.Cl.N1CCNCC1.Br[CH2:22][C:23]1[CH:32]=[CH:31][C:26]([C:27]([O:29][CH3:30])=[O:28])=[CH:25][CH:24]=1>CO>[N:7]1([CH2:22][C:23]2[CH:32]=[CH:31][C:26]([C:27]([O:29][CH3:30])=[O:28])=[CH:25][CH:24]=2)[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1

参加物

5

反応物 3

HCID 8893Piperazine DihydrochlorideHCID 120181Piperazine, hexahydrateHCID 256687Methyl 4-(bromomethyl)benzoate

生成物 1

HCID 7018627Methyl 4-[(piperazin-1-yl)methyl]benzoate収率 64%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixtue of 38 g. (0.2 mole) piperazine hexahydrate, 28 g. (0.2 mole) piperazine dihydrochloride and 150 ml. methanol is mixed, while stirring at ambient temperature, with 45 g. (0.2 mole) methyl 4-bromomethylbenzoate. The reaction mixture is left to stand for 2 days and suction filtered from the precipitate. The clear solution is evaporated and the residue is recrystallised from ethanol to give 39 g. (64%) of the desired compound as a monohydrochloride; m.p. 226°-227° C.

後処理

  1. waitThe reaction mixture is left
  2. filtrationsuction filtered from the precipitate
  3. customThe clear solution is evaporated
  4. customthe residue is recrystallised from ethanol
  5. customto give 39 g

出典と根拠

ORDレコード
ord-c2a1209efed14541a56982e6500c44bc
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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