Hydrochloric Acid → N-(6-benzenesulfonyl-1,2,3,4-tetrahydro-naphthalen-1-yl)-N'-methyl-ethane-1,2-diamine

HRID 2103348노트

반응식

HRID 2103348 반응식
C(O[C:6](=O)[N:7]([CH2:9][CH2:10][NH:11][CH:12]1[C:21]2[C:16](=[CH:17][C:18]([S:22]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)(=[O:24])=[O:23])=[CH:19][CH:20]=2)[CH2:15][CH2:14][CH2:13]1)C)(C)(C)C.Cl>O1CCCC1.CCOCC>[C:25]1([S:22]([C:18]2[CH:17]=[C:16]3[C:21](=[CH:20][CH:19]=2)[CH:12]([NH:11][CH2:10][CH2:9][NH:7][CH3:6])[CH2:13][CH2:14][CH2:15]3)(=[O:23])=[O:24])[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 57804253[2-(6-Benzenesulfonyl-1,2,3,4-tetrahydro-naphthalen-1-ylamino)-ethyl]-methyl-carbamic acid tert-butyl ester

생성물 1

HCID 11523041N-(6-benzenesulfonyl-1,2,3,4-tetrahydro-naphthalen-1-yl)-N'-methyl-ethane-1,2-diamine수율 97%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

[2-(6-Benzenesulfonyl-1,2,3,4-tetrahydro-naphthalen-1-ylamino)-ethyl]-methyl-carbamic acid tert-butyl ester (0.4 g, 0.9 mmol) was dissolved in 20 mL of tetrahydrofuran, and 20 mL of 10% HCl in Et2O was added. The reaction mixture was refluxed for one hour and then cooled. The solvent was evaporated under reduced pressure, and the resulting solid was recrystallized from EtOH-Et2O to yield 0.3 g (0.87 mmol, 97%) of N-(6-benzenesulfonyl-1,2,3,4-tetrahydro-naphthalen-1-yl)-N′-methyl-ethane-1,2-diamine as a hydrochloride salt. MS: 345 (M+H)+.

후처리

  1. temperatureThe reaction mixture was refluxed for one hour
  2. temperaturecooled
  3. customThe solvent was evaporated under reduced pressure
  4. customthe resulting solid was recrystallized from EtOH-Et2O

출처 및 근거

ORD 기록
ord-63fca4eb8c8a49d49282f6213f684e74
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576103B2

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