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Aluminum(III) Chloride → 1-Chloro-7-hydroxy-4-nitro-9H-thioxanthen-9-one

HRID 364209
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반응식

HRID 364209 반응식
[Cl:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[C:11]([O:17]C)[CH:12]=3)[S:7][C:6]=2[C:5]([N+:19]([O-:21])=[O:20])=[CH:4][CH:3]=1.[Cl-].[Al+3].[Cl-].[Cl-]>ClCCCl>[Cl:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[C:11]([OH:17])[CH:12]=3)[S:7][C:6]=2[C:5]([N+:19]([O-:21])=[O:20])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6451240Aluminum(III) ChlorideHCID 13590116HCID 13590116, 화합물

생성물 1

HCID 135901181-Chloro-7-hydroxy-4-nitro-9H-thioxanthen-9-one

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

A mixture of 25 g of 1-chloro-7-methoxy-4-nitro-9H-thioxanthen-9-one, 32.1 g of anhydrous aluminum chloride, and 300 ml of 1,2-dichloroethane is heated under reflux for 1.5 hours. The mixture is concentrated, then treated with 640 ml of concentrated HCl. After 1 hour, the slurry is filtered, and then washed with 500 ml of water followed by 300 ml of 2-propanol, to afford the title compound as a gold solid, mp>300° C.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 1.5 hours
  3. concentrationThe mixture is concentrated
  4. additiontreated with 640 ml of concentrated HCl
  5. filtrationthe slurry is filtered
  6. washwashed with 500 ml of water

출처 및 근거

ORD 기록
ord-51da5aa45f4143d6a249e4d919b938a9
출처 데이터셋
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04604390

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