Water → HCID 86612670、化合物

HRID 1982987ノート

反応式

HRID 1982987 の反応式
Cl[CH2:2][N:3]1[CH:7]=[C:6]([S:8][C:9]([Cl:12])([Cl:11])[F:10])[CH:5]=[N:4]1.[F:13][C:14]([F:23])([F:22])[CH2:15][CH2:16][CH:17]([C:20]#[N:21])[C:18]#[N:19].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[Cl:11][C:9]([Cl:12])([F:10])[S:8][C:6]1[CH:5]=[N:4][N:3]([CH2:2][C:17]([CH2:16][CH2:15][C:14]([F:13])([F:22])[F:23])([C:18]#[N:19])[C:20]#[N:21])[CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 221857612-(3,3,3-Trifluoropropyl)malononitrileHCID 23149146HCID 23149146、化合物

生成物 1

HCID 86612670HCID 86612670、化合物収率 19%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

0.21 g of 1-(chloromethyl)-4-[(dichlorofluoromethyl)thio]-1H-pyrazole and 0.14 g of (3,3,3-trifluoropropyl) malononitrile were dissolved in 2 ml of N,N-dimethylformamide. 0.12 g of potassium carbonate was added to the solution under ice cooling, followed by stirring at room temperature for overnight. Water was added to the reaction mixture, and then extracted with MTBE. The organic layer was washed with water, dried over anhydrous magnesium sulfate, filtered. The filtrate was concentrated under reduced pressure to obtain 0.06 g of [(4-{(dichlorofluoromethyl)thio}-1H-pyrazole-1-yl)methyl](3,3,3-trifluoropropyl)malononitrile (referred as the compound of the present invention (43), hereinafter) shown by below formula.

後処理

  1. extractionextracted with MTBE
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-021a164499164cd8be936aca79678d57
出典データセット
uspto-grants-2009_06
特許番号
US07541374B2

反応ノート

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