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Potassium Carbonate → 4-(5,6-Dichloro-2-methylamino-pyrimidin-4-yl)-piperazine-1-carboxylic acid tert-butyl ester

HRID 2403264
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반응식

HRID 2403264 반응식
[CH3:1][NH:2][C:3]1[N:8]=[C:7](Cl)[C:6]([Cl:10])=[C:5]([Cl:11])[N:4]=1.[C:12]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13].C(=O)([O-])[O-].[K+].[K+]>O.C(C(C)=O)C>[C:15]([O:14][C:12]([N:19]1[CH2:24][CH2:23][N:22]([C:7]2[C:6]([Cl:10])=[C:5]([Cl:11])[N:4]=[C:3]([NH:2][CH3:1])[N:8]=2)[CH2:21][CH2:20]1)=[O:13])([CH3:18])([CH3:16])[CH3:17]
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참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 143452tert-Butyl piperazine-1-carboxylateHCID 15567730Methyl-(4,5,6-trichloro-pyrimidin-2-yl)-amine

생성물 1

HCID 574437034-(5,6-Dichloro-2-methylamino-pyrimidin-4-yl)-piperazine-1-carboxylic acid tert-butyl ester수율 59%

시약·촉매·용매 2

HCID 962Water용매
HCID 6569
Methyl Ethyl Ketone
용매

실험 절차

Methyl-(4,5,6-trichloro-pyrimidin-2-yl)-amine (2.8 g, 12.2 mmol), 1-Boc-piperazine (2.27 g, 12.2 mmol), potassium carbonate (0.84 g 6.1 mmol) in water (2.5 ml) and methyl ethyl ketone (50 ml) were refluxed for 12 hours. After cooling to room temperature the precipitate was filtered, and washed with water to give the title compound (2.6 g, 59%), melting point: 205-206° C.

후처리

  1. filtrationwas filtered
  2. washwashed with water

출처 및 근거

ORD 기록
ord-ec17a0bda749446ab6d0c0f18ef41e54
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08802672B2

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