Sulfuryl chloride → 4-Chloro-5,6,7,8-tetrahydronaphthalen-1-ol

HRID 1076871

반응식

HRID 1076871 반응식
[C:1]1([OH:11])[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.S(Cl)([Cl:15])(=O)=O>C(Cl)(Cl)(Cl)Cl>[Cl:15][C:4]1[C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[C:1]([OH:11])=[CH:2][CH:3]=1

참가 물질

4

반응물 2

HCID 24648Sulfuryl chlorideHCID 682585,6,7,8-Tetrahydro-1-naphthol

생성물 1

HCID 202033334-Chloro-5,6,7,8-tetrahydronaphthalen-1-ol수율 17.5%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

A solution of 37 grams (0.25 mole) of 5,6,7,8-tetrahydronaphthol in 200 ml of carbon tetrachloride was treated dropwise with stirring with 33.8 grams (0.25 mole) of sulfuryl chloride at room temperature. When addition was complete the reaction mixture slowly brought to boiling over a 1 hour period and held there at reflux for 30 minutes. After cooling to ambient temperature the reaction mixture was washed with 10 percent aqueous sodium carbonate and then with water. After drying over calcium chloride the carbon tetrachloride solution was distilled to give a portion, b.p. 110-112/0.25 mm, which was recrystallized from hexane to give 8 grams (17.5 percent) of product, m.p. 58°-59°C.

후처리

  1. additionWhen addition
  2. temperatureat reflux for 30 minutes
  3. washwas washed with 10 percent aqueous sodium carbonate
  4. dry with materialAfter drying over calcium chloride the carbon tetrachloride solution
  5. distillationwas distilled
  6. customto give a portion
  7. custom110-112/0.25 mm, which was recrystallized from hexane

출처 및 근거

ORD 기록
ord-08e7a9c04ba34703be6b3f2656ea7360
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03958006

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