Chloroform → tert-Butyl 4-(bromoacetyl)piperazine-1-carboxylate

HRID 421834노트

반응식

HRID 421834 반응식
[Br:1][CH2:2][C:3](Br)=[O:4].C(Cl)(Cl)Cl.[C:10]([O:14][C:15]([N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1)=[O:16])([CH3:13])([CH3:12])[CH3:11].C(N(CC)CC)C>C(OCC)(=O)C>[Br:1][CH2:2][C:3]([N:20]1[CH2:19][CH2:18][N:17]([C:15]([O:14][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:16])[CH2:22][CH2:21]1)=[O:4]

참가 물질

6

반응물 4

HCID 6212ChloroformHCID 8471TriethylamineHCID 61147Bromoacetyl bromideHCID 143452tert-Butyl piperazine-1-carboxylate

생성물 1

HCID 15829155tert-Butyl 4-(bromoacetyl)piperazine-1-carboxylate

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

With cooling with ice, bromoacetyl bromide (680 μL) was added to a chloroform (10 ml) solution of 1-tert-butyloxycarbonylpiperazine (1 g) and triethylamine (2.2 mL). At that temperature, this was stirred for 0.5 hours, and then at room temperature for further 0.5 hours. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline water, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (hexane/ethyl acetate=7/3) to obtain 340 mg of the entitled compound.

후처리

  1. waitat room temperature for further 0.5 hours
  2. customThe reaction liquid
  3. washwashed with water and saturated saline water
  4. dry with materialdried with anhydrous sodium sulfate
  5. customThe solvent was evaporated away under reduced pressure
  6. customthe resulting residue was purified through silica gel column chromatography (hexane/ethyl acetate=7/3)

출처 및 근거

ORD 기록
ord-416098bc7ea845c8b9890c1bae4291e0
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08101618B2

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