Potassium Carbonate → Tert-butyl 4-benzhydrylpiperazine-1-carboxylate

HRID 1457606

反応式

HRID 1457606 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Br[CH:15]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)P(N(C)C)(N(C)C)=O>O>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH:15]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 12679HexamethylphosphoramideHCID 143452tert-Butyl piperazine-1-carboxylateHCID 236603Bromodiphenylmethane

生成物 1

HCID 4935532Tert-butyl 4-benzhydrylpiperazine-1-carboxylate収率 70.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 3.7 g of N-(tert-butoxycarbonyl)piperazine, 2.5 g of bromodiphenylmethane, 6.9 g of potassium carbonate and 20 ml of hexamethylphosphoramide was stirred at 40° to 50° C. for 4 hours. After cooling, water was added and the reaction mixture was extracted with diethyl ether. The exact was washed and dried, and the solvent was removed under reduced pressure. Hexane was added to the precipitated crystals and the crystals were collected by filtration to give 2.5 g of 4-(tert-butoxycarbonyl)-1-diphenylmethylpiperazine (melting point: 129°-131° C.).

後処理

  1. temperatureAfter cooling
  2. extractionthe reaction mixture was extracted with diethyl ether
  3. washThe exact was washed
  4. customdried
  5. customthe solvent was removed under reduced pressure
  6. additionHexane was added to the precipitated crystals
  7. filtrationthe crystals were collected by filtration

出典と根拠

ORDレコード
ord-07f4804c63e542a694dcb1c822559c1c
出典データセット
uspto-grants-1998_12
特許番号
US05849732

関連ノート

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