Water → 3-Methyl-3-[(4-methylbenzene-1-sulfonyl)methyl]oxetane

HRID 8285

반응식

HRID 8285 반응식
[CH3:1][C:2]1([CH2:6]O)[CH2:5][O:4][CH2:3]1.[OH-].[Na+].[C:10]1([CH3:20])[CH:15]=[CH:14][C:13]([S:16](Cl)(=[O:18])=[O:17])=[CH:12][CH:11]=1.O>C(Cl)Cl>[CH3:1][C:2]1([CH2:6][S:16]([C:13]2[CH:14]=[CH:15][C:10]([CH3:20])=[CH:11][CH:12]=2)(=[O:18])=[O:17])[CH2:5][O:4][CH2:3]1

참가 물질

6

반응물 4

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 14798Sodium HydroxideHCID 1378373-Methyl-3-oxetanemethanol

생성물 1

HCID 220152623-Methyl-3-[(4-methylbenzene-1-sulfonyl)methyl]oxetane

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

3-methyl-3-oxetanemethanol (100 g, 0.98 mol) was dissolved in 250 mL methylene chloride, and a 35% solution of sodium hydroxide (143.60 g, 1.08 mol)was added, and the reaction was cooled to 0° C. A solution of p-toluenesulfonyl chloride was added (186.67 g, 0.98 mol) in 375 mL methylene chloride was added over 1 hour. A white precipitate formed immediately. The reaction was stirred for 10 additional hours. 1000 mL of water was added. The dichloromethane solution layer was then removed, and dried with sodium sulfate, and the solvent was removed. Yield: 217.77 grams of 3-methyl-3-tosylmethyloxetane as white crystals, 87%.

후처리

  1. additionwas added over 1 hour
  2. customA white precipitate formed immediately
  3. customThe dichloromethane solution layer was then removed
  4. dry with materialdried with sodium sulfate
  5. customthe solvent was removed

출처 및 근거

ORD 기록
ord-9c4c3610f2df4ee7bbd50d06f17076ad
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07087710B2

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