Methyl trifluoromethyl ketone → HCID 178465586、化合物

HRID 642602ノート

反応式

HRID 642602 の反応式
[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]

参加物

4

反応物 3

HCID 9871Methyl trifluoromethyl ketoneHCID 5561003-Chloro-2-hydrazinylpyridineHCID 178514363HCID 178514363、化合物

生成物 1

HCID 178465586HCID 178465586、化合物収率 66%

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-93abc894830e46c398d9815e2ab42d12
出典データセット
uspto-grants-2010_04
特許番号
US07696233B2

反応ノート

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