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Potassium Phosphate, Tribasic → 2-Chloro-5-cyclopropylpyrimidine

HRID 40564
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HRID 40564 반응식
Br[C:2]1[CH:3]=[N:4][C:5]([Cl:8])=[N:6][CH:7]=1.[CH:9]1(B(O)O)[CH2:11][CH2:10]1.[O-]P([O-])([O-])=O.[K+].[K+].[K+].C1(P(C2CCCCC2)C2CCCCC2)CCCCC1>CC([O-])=O.CC([O-])=O.[Pd+2].C1(C)C=CC=CC=1.O>[Cl:8][C:5]1[N:4]=[CH:3][C:2]([CH:9]2[CH2:11][CH2:10]2)=[CH:7][N:6]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 62657Potassium Phosphate, TribasicHCID 75806TricyclohexylphosphineHCID 6066655-Bromo-2-chloropyrimidineHCID 2760897Cyclopropylboronic acid

생성물 1

HCID 468640872-Chloro-5-cyclopropylpyrimidine

시약·촉매·용매 3

HCID 167845palladium(II) acetate촉매
이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트
HCID 962
Water
용매
HCID 1140Toluene용매

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온도
100 °C

실험 절차

3.60 g (18.6 mmol) 5-bromo-2-chloropyrimidine, 4.80 g (55.8 mmol) cyclopropyl boronic acid, 13.8 g (65.1 mmol) K3PO4,568 mg (2.03 mmol) tricyclohexylphosphine and 4 mL water are added to 80 mL toluene. The mixture is degassed thoroughly and charged with 627 mg (2.79 mmol) Pd(OAc)2. After degassing again the mixture is stirred at 100° C. over night, filtered and the solvent is removed in vacuo. The crude product is purified by column chromatography (silica gel, PE/EtOAc 90/10→70/30).

후처리

  1. customThe mixture is degassed thoroughly
  2. customAfter degassing again the mixture
  3. filtrationfiltered
  4. customthe solvent is removed in vacuo
  5. customThe crude product is purified by column chromatography (silica gel, PE/EtOAc 90/10→70/30)

출처 및 근거

ORD 기록
ord-61973ad4c4ec4f6fa03b98ec4f2b656c
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08530460B2

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