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Triethylamine → HCID 5181860、化合物

HRID 1643467
ノート
印刷プレビュー

反応式

HRID 1643467 の反応式
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:4]=[C:5]([S:9](Cl)(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1.[NH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH:16]1[CH2:21][OH:22].C(N(CC)CC)C>C(Cl)Cl>[F:1][C:2]([F:14])([F:13])[C:3]1[CH:4]=[C:5]([S:9]([N:15]2[CH2:20][CH2:19][CH2:18][CH2:17][CH:16]2[CH2:21][OH:22])(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 94263Piperidin-2-ylmethanolHCID 27332503-(Trifluoromethyl)benzenesulfonyl chloride

生成物 1

HCID 5181860HCID 5181860、化合物収率 28%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

3-(Trifluoromethyl)benzenesulfonic acid chloride (1 eq), dissolved in methylene chloride (65 ml), was added dropwise to a cooled solution (0° C.) of 2-piperidinemethanol (40 mmol, 1.1 eq) in methylene chloride (160 ml) and triethylamine (2.5 eq). When the addition was complete, the cooling bath was removed and the reaction mixture was stirred at room temperature until, according to thin layer chromatography control, the reaction was complete (90 min). Hydrogen chloride solution (0.5 mol/l, 75 ml) was added, the mixture was stirred for 15 min, the phases were separated and the organic phase was washed with water, dried over sodium sulfate and concentrated in vacuo. Yield: 28%

後処理

  1. additionWhen the addition
  2. customthe cooling bath was removed
  3. custom(90 min)
  4. additionHydrogen chloride solution (0.5 mol/l, 75 ml) was added
  5. stirringthe mixture was stirred for 15 min
  6. customthe phases were separated
  7. washthe organic phase was washed with water
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-b79cbd13708a4a4db28c4391c1e12819
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08119805B2

反応ノート

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