Thionyl Chloride → 1-Chloroisoquinoline-5-sulfonyl chloride hydrochloride

HRID 2118499

반응식

HRID 2118499 반응식
S(Cl)([Cl:3])=O.[Cl:5][C:6]1[C:15]2[CH:14]=[CH:13][CH:12]=[C:11]([S:16]([OH:19])(=O)=[O:17])[C:10]=2[CH:9]=[CH:8][N:7]=1>CN(C)C=O>[ClH:3].[Cl:5][C:6]1[C:15]2[CH:14]=[CH:13][CH:12]=[C:11]([S:16]([Cl:3])(=[O:19])=[O:17])[C:10]=2[CH:9]=[CH:8][N:7]=1

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 137300201-Chloroisoquinoline-5-sulfonic acid

생성물 1

HCID 219799361-Chloroisoquinoline-5-sulfonyl chloride hydrochloride

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To 40 ml of thionyl chloride were added 2.93 g of 1-chloro-5-isoquinolinesulfonic acid as obtained in Example 1 and 0.4 ml of N,N-dimethylformamide. Then, the resulting mixture was refluxed while heating at 80° to 85° C. for 2 hours, followed by removal of the thionyl chloride under reduced pressure. Subsequently, 10 ml of dichloromethane was added to the reaction mixture to precipitate crystals, followed by separation of the crystals by filtration. The crystals thus obtained were washed with 10 ml of dichloromethane, and then dried under reduced pressure to obtain 3.06 g of 1-chloro-5-isoquinolinesulfonyl chloride hydrochloride. The compound was analyzed to give the following data.

후처리

  1. temperatureThen, the resulting mixture was refluxed
  2. temperaturewhile heating at 80° to 85° C. for 2 hours
  3. customfollowed by removal of the thionyl chloride under reduced pressure
  4. additionSubsequently, 10 ml of dichloromethane was added to the reaction mixture
  5. customto precipitate crystals
  6. customfollowed by separation of the crystals by filtration
  7. customThe crystals thus obtained
  8. washwere washed with 10 ml of dichloromethane
  9. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-63a1456ec45c4ca2a3dd72572ef1f150
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04678783

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