1-Bromo-3-chloropropane → N-(3-Chloropropyl)-5,6-dimethoxy-1,2-benzisothiazoline-1,1-dioxide

HRID 259535노트

반응식

HRID 259535 반응식
[CH3:1][O:2][C:3]1[C:4]([O:14][CH3:15])=[CH:5][C:6]2[S:10](=[O:12])(=[O:11])[N:9]=[CH:8][C:7]=2[CH:13]=1.Br[CH2:17][CH2:18][CH2:19][Cl:20]>[OH-].[Na+].C(O)C>[Cl:20][CH2:19][CH2:18][CH2:17][N:9]1[CH2:8][C:7]2[CH:13]=[C:3]([O:2][CH3:1])[C:4]([O:14][CH3:15])=[CH:5][C:6]=2[S:10]1(=[O:12])=[O:11]

참가 물질

5

반응물 2

HCID 80061-Bromo-3-chloropropaneHCID 681175355,6-Dimethoxy-1,2-benzisothiazoline-1,1-dioxide

생성물 1

HCID 53817430N-(3-Chloropropyl)-5,6-dimethoxy-1,2-benzisothiazoline-1,1-dioxide

시약·촉매·용매 2

HCID 702Ethanol용매HCID 14798Sodium Hydroxide용매

실험 절차

2.4 gm (10.5 millimols) of the compound obtained in step (d) were dissolved in a mixture of 15 ml of an aqueous 2.5% sodium hydroxide solution and 30 ml of ethanol, and the solution was refluxed for 8 hours after addition of 10 ml of 3-bromo-1-chloro-propane. The reaction mixture was thereafter evaporated to half its volume, diluted with water and extracted with chloroform. After drying of the organic phase it was evaporated in vacuo, and the desired product was obtained as a highly viscous oil. Rf -value (chloroform/methanol = 19/1: 0.8.

후처리

  1. temperaturethe solution was refluxed for 8 hours
  2. customThe reaction mixture was thereafter evaporated to half its volume
  3. additiondiluted with water
  4. extractionextracted with chloroform
  5. customAfter drying of the organic phase it
  6. customwas evaporated in vacuo

출처 및 근거

ORD 기록
ord-eaa1d893d50349c2b4e40f9b270b2a2a
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04038407

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