4-Benzyl-2,6-dichloropyrimidine → 4-Benzyl-2-chloro-pyrimidine

HRID 1855325노트

반응식

HRID 1855325 반응식
[CH2:1]([C:8]1[N:13]=[C:12]([Cl:14])[N:11]=[C:10](Cl)[CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>N.C(OCC)(=O)C.[Zn]>[CH2:1]([C:8]1[CH:9]=[CH:10][N:11]=[C:12]([Cl:14])[N:13]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 1

HCID 462230714-Benzyl-2,6-dichloropyrimidine

생성물 1

HCID 183533314-Benzyl-2-chloro-pyrimidine수율 102.6%

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 222Ammonia용매HCID 8857Ethyl Acetate용매

반응 조건

온도
20 °C

실험 절차

To an emulsion of 6-benzyl-2,4-dichloro-pyrimidine (239 mg, 1 mmol) in 25% aqueous ammonia solution (1 mL) was added after stirring for 10 min at 0° C. zinc powder (82 mg, 1.25 mmol). The reaction was stirred at 20° C. for 16 h. The yellow suspension was diluted with ethyl acetate an insoluble material was filtered off. The layers were separated and the aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate and evaporated under reduced pressure to yield the crude title compound (210 mg, 92%) as a yellow oil.

후처리

  1. filtrationwas filtered off
  2. customThe layers were separated
  3. extractionthe aqueous layer was extracted with ethyl acetate
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over sodium sulfate
  6. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-c51372fc5ba742a7b6bf8c65b587339b
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962834B2

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