Triethylamine → Benzyl 4-(4-bromophenyl)piperazine-1-carboxylate

HRID 41693

反応式

HRID 41693 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.C(N(CC)CC)C.Cl[C:22]([O:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:23]>ClCCl>[CH2:25]([O:24][C:22]([N:11]1[CH2:12][CH2:13][N:8]([C:5]2[CH:4]=[CH:3][C:2]([Br:1])=[CH:7][CH:6]=2)[CH2:9][CH2:10]1)=[O:23])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10387Benzyl chloroformateHCID 27356291-(4-Bromophenyl)piperazine

生成物 1

HCID 46739494Benzyl 4-(4-bromophenyl)piperazine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

5 g of 4-bromophenylpiperazine are placed in a 500 ml three-necked flask under a nitrogen atmosphere. 4.34 ml of triethylamine are added. The mixture is cooled in an ice bath and 3.24 ml of benzyl chloroformate are added. The mixture is allowed to return to ambient temperature. It is diluted with dichloromethane and then gentle hydrolysis is carried out. The aqueous phase is extracted with dichloromethane. The organic phases are combined, washed with a saturated NaCl solution, dried over sodium sulphate, then filtered through a sintered glass filter and concentrated under vacuum. 8.43 g of 4-(4-bromophenyl)piperazine-1-carboxylic acid benzyl ester are obtained.

後処理

  1. temperatureThe mixture is cooled in an ice bath
  2. customto return to ambient temperature
  3. customgentle hydrolysis
  4. extractionThe aqueous phase is extracted with dichloromethane
  5. washwashed with a saturated NaCl solution
  6. dry with materialdried over sodium sulphate
  7. filtrationfiltered through a sintered glass
  8. filtrationfilter
  9. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-c53fbf5f16654f649222fece5a7bfb47
出典データセット
uspto-grants-2013_09
特許番号
US08530657B2

関連ノート

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