Pyridine → 3-Methyl-3-(toluenesulfonyl-oxymethyl)oxetane

HRID 1009301

反応式

HRID 1009301 の反応式
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7](Cl)(=[O:9])=[O:8])=[CH:3][CH:2]=1.[CH3:12][C:13]1([CH2:17][OH:18])[CH2:16][O:15][CH2:14]1.N1C=CC=C[CH:20]=1>>[CH3:12][C:13]1([CH2:17][O:18][S:7]([C:4]2[C:5]([CH3:20])=[CH:6][CH:1]=[CH:2][CH:3]=2)(=[O:8])=[O:9])[CH2:16][O:15][CH2:14]1.[S:7]([C:4]1[CH:5]=[CH:6][C:1]([CH3:11])=[CH:2][CH:3]=1)([OH:15])(=[O:9])=[O:8].[O:15]1[CH2:16][CH2:13][CH2:14]1

参加物

5

反応物 3

HCID 1049PyridineHCID 73974-Toluenesulfonyl chlorideHCID 1378373-Methyl-3-oxetanemethanol

生成物 2

HCID 534258303-Methyl-3-(toluenesulfonyl-oxymethyl)oxetaneHCID 86590555Oxetane tosylate

実験手順

p-Toluenesulfonyl chloride (57.2 g, 300 mmol) was dissolved in dry pyridine (400 mL) under nitrogen atmosphere. 3-methyl-3-(hydroxymethyl)oxetane (20.4 g, 200 mmol) was added slowly, and the solution was stirred for 1.5 h. Crushed ice (400 g) was then added to vigorously stirring mixture, which was allowed to stir for an additional 0.5 h. The white precipitate was then collected on Whatman filter paper #1 and washed with cold water. The product was dried under high vacuum to obtain 3-methyl-3-(toluenesulfonyl-oxymethyl)oxetane (oxetane tosylate) as a white powder of oxetane tosylate.

後処理

  1. stirringto vigorously stirring mixture, which
  2. stirringto stir for an additional 0.5 h
  3. customThe white precipitate was then collected on Whatman
  4. filtrationfilter paper #1
  5. washwashed with cold water
  6. customThe product was dried under high vacuum

出典と根拠

ORDレコード
ord-c9c2d0b8e8c04da68d2579acf262ee4f
出典データセット
uspto-grants-2011_07
特許番号
US07973037B2

関連ノート

読み込み中…