Potassium thiocyanate → HCID 59386313, 화합물

HRID 1969517노트

반응식

HRID 1969517 반응식
[CH3:1][C:2]1([S:5]([O:8]CCCC)(=[O:7])=[O:6])[CH2:4][CH2:3]1.[S-]C#N.[K+:16]>O1CCOCC1.O>[CH3:1][C:2]1([S:5]([O-:8])(=[O:7])=[O:6])[CH2:4][CH2:3]1.[K+:16]

참가 물질

4

반응물 2

HCID 516872Potassium thiocyanateHCID 58133073Butyl 1-methylcyclopropane-1-sulfonate

생성물 1

HCID 59386313HCID 59386313, 화합물

시약·촉매·용매 1

HCID 218864351,4-Dioxane--water (1/1)용매

실험 절차

A mixture of butyl 1-methylcyclopropane-1-sulfonate (0.80 g, 4.2 mmol) and potassium thiocyanate (0.404 g, 4.16 mmol) in 1,4-dioxane/water (1:1, 10 mL) was heated at reflux for about 8 h. The reaction was cooled to ambient temperature and the solvents were concd under reduced pressure to yield crude potassium 1-methylcyclopropane-1-sulfonate which was suspended in thionyl chloride (7 mL). DMF (0.05 mL) was added and the mixture was heated at reflux for about 8 h and then cooled. The volatiles were removed under reduced pressure and the residue was dissolved in DCM (20 mL), washed with water (15 mL), dried over anhydrous MgSO4 and concd under reduced pressure to yield 1-methylcyclopropane-1-sulfonyl chloride (0.56 g, 86%) as a yellow oil. 1H NMR (DMSO-d6) δ 1.82 (br s, 2H), 1.79 (s, 3H), 1.15 (m, 2H).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for about 8 h

출처 및 근거

ORD 기록
ord-3f777f26663b4d41a3a4b5a11529ac69
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08426411B2

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