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Ammonium Chloride → HCID 68551762、化合物

HRID 1868050
ノート
印刷プレビュー

反応式

HRID 1868050 の反応式
[C:1]1([S:7]([CH:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:17]1[C:22]([C:23]([F:26])([F:25])[F:24])=[CH:21][CH:20]=[CH:19][N:18]=1.C(N(C(C)C)CC)(C)C.[NH4+].[Cl-]>O1CCOCC1>[C:1]1([S:7]([CH:10]2[CH2:11][CH2:12][N:13]([C:17]3[C:22]([C:23]([F:26])([F:25])[F:24])=[CH:21][CH:20]=[CH:19][N:18]=3)[CH2:14][CH2:15]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
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 25517Ammonium ChlorideHCID 81531DiisopropylethylamineHCID 5898332-Chloro-3-(trifluoromethyl)pyridineHCID 5190868HCID 5190868、化合物

生成物 1

HCID 68551762HCID 68551762、化合物収率 55%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a microwave vial were charged 4-(phenylsulfonyl)piperidine (300 mg, 1.33 mmol), 2-chloro-3-(trifluoromethyl)pyridine, (484 mg, 2.66 mmol), diisopropylethylamine (0.695 mL, 3.99 mmol) and 1,4-Dioxane (0.2 mL). The reaction mixture thus prepared was irradiated at 200° C. for 1 hour. The reaction was complete as determined by TLC. The residue was added with saturated NH4Cl (aq.) and extracted with ethylacetate, washed with 10% HCl (aq.), water then brine. Organic layer was dried over MgSO4. Solvent evaporation afforded 2-[4-(phenylsulfonyl)piperidin-1-yl]-3-(trifluoromethyl)pyridine in 55% yield (270 mg) as white solid.

後処理

  1. customThe reaction mixture thus prepared
  2. customwas irradiated at 200° C. for 1 hour
  3. extractionextracted with ethylacetate
  4. washwashed with 10% HCl (aq.), water
  5. dry with materialOrganic layer was dried over MgSO4
  6. customSolvent evaporation

出典と根拠

ORDレコード
ord-570587f1a97d462da435cce6022d79cd
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07632838B2

反応ノート

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