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Triethylamine → N-[1-(2,4-dichlorophenyl)-1-methoxypropan-2-yl]-3-(difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carboxamide

HRID 589302
ノート
印刷プレビュー

反応式

HRID 589302 の反応式
[F:1][CH:2]([F:13])[C:3]1[C:7]([C:8](Cl)=[O:9])=[C:6]([F:11])[N:5]([CH3:12])[N:4]=1.[Cl:14][C:15]1[CH:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:16]=1[CH:22]([O:26][CH3:27])[CH:23]([NH2:25])[CH3:24].C(N(CC)CC)C.C(OCC)(=O)C>ClCCl>[Cl:14][C:15]1[CH:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:16]=1[CH:22]([O:26][CH3:27])[CH:23]([NH:25][C:8]([C:7]1[C:3]([CH:2]([F:13])[F:1])=[N:4][N:5]([CH3:12])[C:6]=1[F:11])=[O:9])[CH3:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 529205085-fluoro-1-methyl-3-difluoromethyl-1H-pyrazole-4-carbonyl chlorideHCID 594032951-(2,4-Dichlorophenyl)-1-methoxypropan-2-amine

生成物 1

HCID 67963548N-[1-(2,4-dichlorophenyl)-1-methoxypropan-2-yl]-3-(difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carboxamide収率 97.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

At ambient temperature, 233 mg (1.1 mmol) of 3-(difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carbonyl chloride and 234 mg (1 mmol) of 1-(2,4-dichlorophenyl)-1-methoxypropan-2-amine are dissolved in 10 ml of dichloromethane. 121 mg (1.2 mmol) of triethylamine are added and the reaction mixture is stirred for 4 hrs at ambient temperature. The mixture is diluted by 50 ml of ethyl acetate and successively washed by a 1 N solution of HCl (twice), a saturated solution of potassium carbonate (twice) and brine and dried over magnesium sulfate. The solvents are removed and the crude amide is purified by column chromatography on silica gel (gradient heptane/ethyl acetate) to yields 400 mg (97% yield) of N-[1-(2,4-dichlorophenyl)-1-methoxypropan-2-yl]-3-(difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carboxamide as a pale yellow solid (M+H=410).

後処理

  1. washsuccessively washed by a 1 N solution of HCl (twice), a saturated solution of potassium carbonate (twice) and brine
  2. dry with materialdried over magnesium sulfate
  3. customThe solvents are removed
  4. customthe crude amide is purified by column chromatography on silica gel (gradient heptane/ethyl acetate)

出典と根拠

ORDレコード
ord-70adf4c7930c4a1f822d953fccfe7f3f
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09232799B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート