Imidazole → 2-Imidazolyl-4,6-dichloropyrimidine

HRID 23183

반응식

HRID 23183 반응식
[NH:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.Cl[C:7]1[C:8]([Cl:14])=[N:9][C:10](Cl)=[N:11][CH:12]=1.C(N(CC)CC)C.[Cl-:22].[NH4+]>C1COCC1>[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:10]1[N:11]=[C:12]([Cl:22])[CH:7]=[C:8]([Cl:14])[N:9]=1

참가 물질

6

반응물 4

HCID 795ImidazoleHCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 2372592,4,5-Trichloropyrimidine

생성물 1

HCID 221700012-Imidazolyl-4,6-dichloropyrimidine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

One equivalent of imidazole is added in one portion to a solution of one equivalent of trichloropyrimidine and 1.5 equivs of triethylamine in THF. After reaction is complete, the reaction mixture is poured into saturated, aqueous ammonium chloride and extracted three times with ethyl acetate. The combined organic layers are washed with brine and dried. The reaction mixture is filtered and all volatiles removed under reduced pressure. The product, 2-imidazolyl-4,6-dichloropyrimidine (the compound of formula (VIIIa)) is isolated by flash chromatography (20% ethyl acetate in hexane) as an off-white solid.

후처리

  1. customAfter reaction
  2. extractionextracted three times with ethyl acetate
  3. washThe combined organic layers are washed with brine
  4. customdried
  5. filtrationThe reaction mixture is filtered
  6. customall volatiles removed under reduced pressure

출처 및 근거

ORD 기록
ord-e92879e3496d4112afd23c6d1dc6781a
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06849739B2

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