Hydrogen Bromide → N-[4-[4-(ethylheptylamino)butyl]phenyl]methanesulfonamide monohydrobromide

HRID 1589347

반응식

HRID 1589347 반응식
[CH2:1]([N:3]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[CH2:4][CH2:5][CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[CH:10][CH:9]=1)[CH3:2].[BrH:26]>C(OCC)C>[BrH:26].[CH2:1]([N:3]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[CH2:4][CH2:5][CH2:6][CH2:7][C:8]1[CH:9]=[CH:10][C:11]([NH:14][S:15]([CH3:18])(=[O:16])=[O:17])=[CH:12][CH:13]=1)[CH3:2]

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 9864094N-(4-(4-(Ethylheptylamino)butyl)phenyl)methanesulfonamide

생성물 1

HCID 70387710N-[4-[4-(ethylheptylamino)butyl]phenyl]methanesulfonamide monohydrobromide수율 37%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

N-[4-[4-(ethylheptylamino)butyl]phenyl]methanesulfonamide (5.56 g, 0.015 mol), prepared according to the general procedure outlined in Example 1, was dissolved in diethyl ether. The solution was cooled with a dry ice/acetone bath and diethyl ether saturated with hydrogen bromide gas was added thereto. The volatiles were evaporated under reduced pressure and 100 ml of ethyl acetate was added to the residue. The solution was triturated and appoximately 6 grams of crystals were collected. The solid was recrystallized from isopropyl alcohol to provide 2.5 g of N-[4-[4-(ethylheptylamino)butyl]phenyl]methanesulfonamide monohydrobromide. mp=98°-100° C. Yield 37%

후처리

  1. temperatureThe solution was cooled with a dry ice/acetone bath
  2. customThe volatiles were evaporated under reduced pressure and 100 ml of ethyl acetate
  3. additionwas added to the residue
  4. customThe solution was triturated
  5. customappoximately 6 grams of crystals were collected
  6. customThe solid was recrystallized from isopropyl alcohol

출처 및 근거

ORD 기록
ord-6d749e6c337e414abdd3df98d3452654
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04569801

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