(2,2-Dimethyl-1,3-dithiolan-4-yl)methanol → 1,3-Dithiolane, 4-(chloromethyl)-2,2-dimethyl-
반응식
[CH3:1][C:2]1([CH3:9])[S:6][CH:5]([CH2:7]O)[CH2:4][S:3]1.S(Cl)([Cl:12])=O>C1(C)C=CC=CC=1>[Cl:12][CH2:7][CH:5]1[CH2:4][S:3][C:2]([CH3:9])([CH3:1])[S:6]1참가 물질
4
실험 절차
To a solution of 3.46 g (0.021 mole) of 2,2-dimethyl-4-hydroxymethyl-1,3-dithiolan in 15 mL of toluene was added dropwise 2.35 g (0.020 mole) of thionyl chloride, and the mixture was heated gradually to 80°-85° C., maintained at that temperature for 0.75 hour, then stirred at room temperature for 16 hours. The mixture was filtered, and the filtrate concentrated to dryness at 60° C./100 mm Hg to give a residual oil. Distillation of the oil gave 1.81 g of product, bp 75°-78° C./1.25-1.35 mm Hg.
후처리
- temperaturethe mixture was heated gradually to 80°-85° C.
- temperaturemaintained at that temperature for 0.75 hour
- filtrationThe mixture was filtered
- concentrationthe filtrate concentrated to dryness at 60° C./100 mm Hg
- customto give a residual oil
- distillationDistillation of the oil
출처 및 근거
- ORD 기록
- ord-0669c09553f140b38c9ed133c4840ed6
- 출처 데이터셋
- uspto-grants-1987_10
- 특허 번호
- US04702763
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