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Cyclobutanone → N-cyclobutylidene-2-methylpropane-2-sulfinamide

HRID 1777308
ノート
印刷プレビュー

反応式

HRID 1777308 の反応式
[C:1]1(=O)[CH2:4][CH2:3][CH2:2]1.[C:6]([S:10]([NH2:12])=[O:11])([CH3:9])([CH3:8])[CH3:7]>O1CCCC1.[O-]CC.[Ti+4].[O-]CC.[O-]CC.[O-]CC>[C:1]1(=[N:12][S:10]([C:6]([CH3:9])([CH3:8])[CH3:7])=[O:11])[CH2:4][CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14496CyclobutanoneHCID 3382465Tert-Butanesulfinamide

生成物 1

HCID 67250305N-cyclobutylidene-2-methylpropane-2-sulfinamide収率 77%

試薬・触媒・溶媒 2

HCID 76524Titanium tetraethoxide触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of titanium (IV) ethoxide (22.4 mL, 107 mmol) and cyclobutanone (5.37 mL, 71.0 mmoL) in tetrahydrofuran (120 mL) was stirred for 10 minutes. Tert-butanesulfinamide (7.17 g, 59.0 mmol) was added and the reaction mixture was stirred at room temperature for 18 hours. The mixture was concentrated and the residue dissolved in ethyl acetate. The solution was washed with saturated aqueous sodium hydrogen carbonate, dried over sodium sulphate and concentrated to give N-cyclobutylidene-2-methylpropane-2-sulfinamide (9.51 g, 77%) as a pale yellow oil which was used directly without purification.

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

後処理

  1. stirringthe reaction mixture was stirred at room temperature for 18 hours
  2. concentrationThe mixture was concentrated
  3. dissolutionthe residue dissolved in ethyl acetate
  4. washThe solution was washed with saturated aqueous sodium hydrogen carbonate
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-0509ea5a3abc4969b1f3e02682985741
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09266857B2

反応ノート

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