Methyl trifluoromethyl ketone → HCID 178465586, 화합물

HRID 475472

반응식

HRID 475472 반응식
[F:1][C:2]([F:7])([F:6])[C:3]([CH3:5])=O.[Cl:8][C:9]1[C:10](=[N:15][NH2:16])[NH:11][CH:12]=[CH:13][CH:14]=1>>[F:1][C:2]([F:7])([F:6])[C:3](=[N:16][N:15]=[C:10]1[C:9]([Cl:8])=[CH:14][CH:13]=[CH:12][NH:11]1)[CH3:5]

참가 물질

4

반응물 3

HCID 9871Methyl trifluoromethyl ketoneHCID 5561003-Chloro-2-hydrazinylpyridineHCID 178514363HCID 178514363, 화합물

생성물 1

HCID 178465586HCID 178465586, 화합물수율 66%

실험 절차

1,1,1-Trifluoroacetone (7.80 g, 69.6 mmol) was added to 3-chloro-2(1H)-pyridinone hydrazone (alternatively named (3-chloro-pyridin-2-yl)-hydrazine) (10 g, 69.7 mmol) at 20-25° C. After the addition was complete, the mixture was stirred for about 10 minutes. The solvent was removed under reduced pressure and the mixture partitioned between ethyl acetate (100 mL) and saturated aqueous sodium carbonate solution (100 mL). The organic layer was dried and evaporated. Chromatography on silica gel (eluted with ethyl acetate) gave the product as an off-white solid (11 g, 66% yield), m.p. 64-64.5° C. (after crystallization from ethyl acetate/hexanes).

후처리

  1. additionAfter the addition
  2. customThe solvent was removed under reduced pressure
  3. customthe mixture partitioned between ethyl acetate (100 mL) and saturated aqueous sodium carbonate solution (100 mL)
  4. customThe organic layer was dried
  5. customevaporated
  6. customChromatography on silica gel (eluted with ethyl acetate) gave

출처 및 근거

ORD 기록
ord-04b594d8bf0244ff84d23de07acb0f5c
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637552B2

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