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Ethyl Acetate → 1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-5-[N-(ethylsulfinylpropyl)-N-methylamino]-4-trifluoromethylsulfonylpyrazole

HRID 2109916
ノート
印刷プレビュー

反応式

HRID 2109916 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[Cl:12][C:13]1[CH:18]=[C:17]([C:19]([F:22])([F:21])[F:20])[CH:16]=[C:15]([Cl:23])[C:14]=1[N:24]1[C:28]([N:29]([CH2:31][CH2:32][CH2:33][S:34][CH2:35][CH3:36])[CH3:30])=[C:27]([S:37]([C:40]([F:43])([F:42])[F:41])(=[O:39])=[O:38])[C:26]([C:44]#[N:45])=[N:25]1.C(=O)(O)[O-].[Na+].C(OCC)(=O)C>ClCCCl>[Cl:23][C:15]1[CH:16]=[C:17]([C:19]([F:22])([F:21])[F:20])[CH:18]=[C:13]([Cl:12])[C:14]=1[N:24]1[C:28]([N:29]([CH2:31][CH2:32][CH2:33][S:34]([CH2:35][CH3:36])=[O:9])[CH3:30])=[C:27]([S:37]([C:40]([F:43])([F:42])[F:41])(=[O:38])=[O:39])[C:26]([C:44]#[N:45])=[N:25]1
参加物反応条件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 8857Ethyl AcetateHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 866002291-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-5-[N-(3-ethylthiopropyl)-N-methylamino]-4-trifluoromethylsulfonylpyrazole

生成物 1

HCID 866002301-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-5-[N-(ethylsulfinylpropyl)-N-methylamino]-4-trifluoromethylsulfonylpyrazole

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
2.5 °C

実験手順

m-Chloroperbenzoic acid (0.091 g, 77%, 0.4 mmol) was added to a solution of 1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-5-[N-(3-ethylthiopropyl)-N-methylamino]-4-trifluoromethylsulfonylpyrazole (0.23 g, 0.4 mmol) in 1,2-dichloroethane at 0-5° C. The mixture was stirred at 0-5° C. for 0.5 hour, then poured into saturated sodium bicarbonate and ethyl acetate. The organic layer was washed with brine, dried (sodium sulfate), evaporated and chromatographed on silica gel eluting with heptane-ethyl acetate (1/1 to 3/7) to give 1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-5-[N-(ethylsulfinylpropyl)-N-methylamino]-4-trifluoromethylsulfonylpyrazole as a light brown oil (Compound number 2-15, 0.186 g, 71%),19F: −63.8, −78.7.

後処理

  1. washThe organic layer was washed with brine
  2. dry with materialdried (sodium sulfate)
  3. customevaporated
  4. customchromatographed on silica gel eluting with heptane-ethyl acetate (1/1 to 3/7)

出典と根拠

ORDレコード
ord-b3c0a70bfaa14c04bc5f6502e5d6d8a5
出典データセット
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07517877B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート