Water → 2-Chloroethyl cycloheptyl sulfide

HRID 2186371

반응식

HRID 2186371 반응식
S(Cl)([Cl:3])=O.[CH:5]1([S:12][CH2:13][CH2:14]O)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1.O.C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl>[CH:5]1([S:12][CH2:13][CH2:14][Cl:3])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1

참가 물질

6

반응물 4

HCID 962WaterHCID 24386Thionyl ChlorideHCID 516892Sodium BicarbonateHCID 224540732-Hydroxyethyl cycloheptyl sulfide

생성물 1

HCID 224533722-Chloroethyl cycloheptyl sulfide

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

5.11 cm3 of thionyl chloride were added dropwise, with stirring and under an inert atmosphere, at a temperature in the region of 20° C. to a solution of 1.74 g of 2-hydroxyethyl cycloheptyl sulfide in 30 cm3 of chloroform. After the addition, the reaction mixture was first stirred for 15 minutes at the same temperature and then for 1 hour at a temperature in the region of 600° C. The mixture was evaporated to dryness under reduced pressure (5 kPa) at a temperature in the region of 40° C., then the residue obtained was taken up with 2 times 50 cm3 of water and then 1 times 50 cm3 of a saturated sodium hydrogencarbonate solution. The ethereal solution, separated by settling, was dried over magnesium sulfate, filtered, and then concentrated under reduced pressure (5 kPa) at a temperature in the region of 400° C. 1.89 g of 2-chloroethyl cycloheptyl sulfide were obtained in the form of an oil.

후처리

  1. additionAfter the addition
  2. waitfor 1 hour at a temperature in the region of 600° C
  3. customThe mixture was evaporated to dryness under reduced pressure (5 kPa) at a temperature in the region of 40° C.
  4. customthe residue obtained
  5. customThe ethereal solution, separated
  6. dry with materialwas dried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure (5 kPa) at a temperature in the region of 400° C

출처 및 근거

ORD 기록
ord-5bba703f4386438b9fc443649848a383
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06403610B1

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