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Hydrochloric Acid → 5-chloro-3-methylthio-5H-dibenzo[a,d]cycloheptene

HRID 2071745
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반응식

HRID 2071745 반응식
[CH3:1][S:2][C:3]1[CH:4]=[CH:5][C:6]2[CH:12]=[CH:11][C:10]3[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=3[CH:8](O)[C:7]=2[CH:18]=1.[ClH:19]>O1CCOCC1>[Cl:19][CH:8]1[C:7]2[CH:18]=[C:3]([S:2][CH3:1])[CH:4]=[CH:5][C:6]=2[CH:12]=[CH:11][C:10]2[CH:13]=[CH:14][CH:15]=[CH:16][C:9]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 202322443-methylthio-5H-dibenzo[a,d]cyclohepten-5-ol

생성물 1

HCID 202322695-chloro-3-methylthio-5H-dibenzo[a,d]cycloheptene

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A solution of 18 g. (0.071 mole) of 3-methylmercapto-5H-dibenzo[a,d]cyclohepten-5-ol in 90 ml. of dry dioxane is cooled in an ice-bath and saturated with dry hydrogen chloride. A solid separates and when precipitation appears to be complete, the mixture is stirred with 150 ml. of petroleum ether and the product collected, washed with petroleum ether, and dried in a vacuum desiccator over potassium hydroxide. The yield of 5-chloro-3-methylmercapto-5H-dibenzo[a,d]cycloheptene is 16 g. (84%), m.p. 135°-138° C. The melting point is unchanged by recrystallization from cyclohexane.

후처리

  1. customA solid separates and when precipitation
  2. customof petroleum ether and the product collected
  3. washwashed with petroleum ether
  4. dry with materialdried in a vacuum desiccator over potassium hydroxide
  5. customThe melting point is unchanged by recrystallization from cyclohexane

출처 및 근거

ORD 기록
ord-f1e1ba1c875c4bf2a20976e1f687871e
출처 데이터셋
uspto-grants-1977_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04048223

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