Trifluoroacetic acid → HCID 11957741、化合物

HRID 655942ノート

反応式

HRID 655942 の反応式
[Cl:1][C:2]1[C:3]([CH:9]2[CH2:11][CH:10]2[N:12]([C:20]([C:22]2[C:23]([CH:28]([F:30])[F:29])=[N:24][N:25]([CH3:27])[CH:26]=2)=[O:21])C(=O)OC(C)(C)C)=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1.FC(F)(F)C(O)=O>ClCCl>[Cl:1][C:2]1[C:3]([CH:9]2[CH2:11][CH:10]2[NH:12][C:20]([C:22]2[C:23]([CH:28]([F:30])[F:29])=[N:24][N:25]([CH3:27])[CH:26]=2)=[O:21])=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 66918177HCID 66918177、化合物

生成物 1

HCID 11957741HCID 11957741、化合物収率 85.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

0.200 g of tert-butyl [2-(3,5-dichloropyridin-2-yl)cyclopropyl]{[3-(difluoromethyl)-1-methyl-1H-pyrazol-4-yl]carbonyl}carbamate (0.00039 mol) are dissolved in 5 ml of dichloromethane. 0.50 ml of trifluoroacetic acid are added to the reaction mixture which is left stirring at room temperature overnight. The reaction mixture is quenched with 15 ml of an aqueous solution of saturated sodium bicarbonate. After separation, the aqueous phase is extracted with dichloromethane (10 ml). The combined organic phases are dried over magnesium sulfate, filtered, concentrated to dryness and purified on silica to yield to 120 mg of N-[2-(3,5-dichloropyridin-2-yl)cyclopropyl]-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxamide (76%).

後処理

  1. waitis left
  2. customThe reaction mixture is quenched with 15 ml of an aqueous solution of saturated sodium bicarbonate
  3. customAfter separation
  4. extractionthe aqueous phase is extracted with dichloromethane (10 ml)
  5. dry with materialThe combined organic phases are dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness
  8. custompurified on silica

出典と根拠

ORDレコード
ord-9dc09ef4331b4d809ec72c88cabcdfeb
出典データセット
uspto-grants-2011_12
特許番号
US08071629B2

反応ノート

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