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(Trifluoromethyl)trimethylsilane → Tert-butyl 4-hydroxy-4-(trifluoromethyl)piperidine-1-carboxylate

HRID 1829184
ノート
印刷プレビュー

反応式

HRID 1829184 の反応式
[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[F:19][C:20]([Si](C)(C)C)([F:22])[F:21].[O:27]=[C:28]1[CH2:33][CH2:32][N:31]([C:34]([O:36][C:37]([CH3:40])([CH3:39])[CH3:38])=[O:35])[CH2:30][CH2:29]1>O1CCCC1>[OH:27][C:28]1([C:20]([F:22])([F:21])[F:19])[CH2:29][CH2:30][N:31]([C:34]([O:36][C:37]([CH3:40])([CH3:39])[CH3:38])=[O:35])[CH2:32][CH2:33]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 552549(Trifluoromethyl)trimethylsilaneHCID 735900tert-Butyl 4-oxopiperidine-1-carboxylateHCID 2724141Tetrabutylammonium Fluoride

生成物 1

HCID 22061329Tert-butyl 4-hydroxy-4-(trifluoromethyl)piperidine-1-carboxylate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Tetrabutylammonium fluoride (50 mg, 1M solution in tetrahydrofuran) was added to an ice-cooled solution of (trifluoromethyl)trimethylsilane (2.1 g, 15 mmol) and tert-butyl 4-oxo-1-piperidinecarboxylate (2 g, 10 mmol) in tetrahydrofuran (20 ml), and the reaction stirred at room temperature for 18 hours. The mixture was concentrated under reduced pressure, the residue suspended in ethyl acetate, hydrochloric acid (20 ml, 1N) was added, the mixture stirred for an hour, and then neutralised using sodium bicarbonate. The solution was washed with water, then brine, dried (MgSO4) and evaporated under reduced pressure to give a gum. This was purified by column chromatography on silica gel using an elution gradient of dichloromethane:methanol (100:0 to 98:2) to afford the title compound, 1.94 g.

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. additionhydrochloric acid (20 ml, 1N) was added
  3. stirringthe mixture stirred for an hour
  4. washThe solution was washed with water
  5. dry with materialbrine, dried (MgSO4)
  6. customevaporated under reduced pressure
  7. customto give a gum
  8. customThis was purified by column chromatography on silica gel using an elution gradient of dichloromethane:methanol (100:0 to 98:2)

出典と根拠

ORDレコード
ord-81dce53ab7e5409aa85e12d3ea7d318b
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07060836B2

反応ノート

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