Methanol → HCID 44198699, 화합물

HRID 1957909노트

반응식

HRID 1957909 반응식
Cl[C:2]1[N:3]=[N:4][C:5]([CH3:24])=[C:6]([C:17]2[CH:18]=[N:19][C:20]([Cl:23])=[CH:21][CH:22]=2)[C:7]=1[C:8]1[C:13]([F:14])=[CH:12][C:11]([F:15])=[CH:10][C:9]=1[F:16].[CH3:25][O-:26].[Na+].CO>O>[Cl:23][C:20]1[N:19]=[CH:18][C:17]([C:6]2[C:7]([C:8]3[C:13]([F:14])=[CH:12][C:11]([F:15])=[CH:10][C:9]=3[F:16])=[C:2]([O:26][CH3:25])[N:3]=[N:4][C:5]=2[CH3:24])=[CH:22][CH:21]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 10942334Sodium MethoxideHCID 44129705HCID 44129705, 화합물

생성물 1

HCID 44198699HCID 44198699, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 3-chloro-5-(6-chloro-pyridin-3-yl)-6-methyl-4-(2,4,6-trifluorophenyl)-pyridazine (Compound No. I.a.11, 700 mg), sodium methoxide (30% solution in methanol, 750 mg) and 10 ml of methanol is heated for 6 h to 60° C. Subsequently the reaction mixture is cooled, diluted with water and extracted with ethyl acetate. The combined organic layer is washed with water and brine, dried over sodium sulfate and evaporated under reduced pressure. The remainder is purified by chromatography on silica gel, using a mixture of heptane/ethyl acetate 3:1 as eluent to obtain 4-(6-chloro-pyridin-3-yl)-6-methoxy-3-methyl-5-(2,4,6-trifluoro-phenyl)-pyridazine (Compound I.a.12), m.p. 123-124° C.

후처리

  1. temperatureis heated for 6 h to 60° C
  2. temperatureSubsequently the reaction mixture is cooled
  3. extractionextracted with ethyl acetate
  4. washThe combined organic layer is washed with water and brine
  5. dry with materialdried over sodium sulfate
  6. customevaporated under reduced pressure
  7. customThe remainder is purified by chromatography on silica gel
  8. additiona mixture of heptane/ethyl acetate 3:1 as eluent

출처 및 근거

ORD 기록
ord-5d5588c4844b47b88d84e95687879996
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08410026B2

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