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

HRID 41693

반응식

HRID 41693 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c53fbf5f16654f649222fece5a7bfb47
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530657B2

연결된 노트

불러오는 중…