Thionyl Chloride → HCID 43620016、化合物
反応式
[O:1]=[S:2]1(=[O:10])[CH2:6][CH2:5][CH2:4][N:3]1[CH2:7][CH2:8]O.O=S(Cl)[Cl:13].C([O-])(O)=O.[Na+]>C(Cl)Cl>[Cl:13][CH2:8][CH2:7][N:3]1[CH2:4][CH2:5][CH2:6][S:2]1(=[O:10])=[O:1]参加物
5
反応条件
- 温度
- 40 °C
実験手順
To a solution of 2-(1,1-dioxo-1λ6-isothiazolidin-2-yl)-ethanol (0.14 g, 0.847 mmol) in DCM (4 mL) was added SOCl2 (0.151 g, 1.27 mmol) and the reaction mixture was heated to 40° C. for 2 h. The mixture was cooled to room temperature, diluted with DCM, poured into a sat. NaHCO3 solution (10 mL) and the aqueous layer was extracted with DCM (2×20 mL). Combined organics were dried over Na2SO4, filtered and evaporated to dryness to give the title compound (0.046 g, 30%) as an orange oil which was used with no further purification. MS: 184.1 (M+H+).
後処理
- temperatureThe mixture was cooled to room temperature
- extractionthe aqueous layer was extracted with DCM (2×20 mL)
- dry with materialCombined organics were dried over Na2SO4
- filtrationfiltered
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-b3357f9e8b9c47ffbc75a78debee8ec8
- 出典データセット
- uspto-grants-2016_02
- 特許番号
- US09260408B2
反応ノート
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