1-Chloro-2-(diethylamine)ethane hydrochloride → HCID 178464092, 화합물

HRID 2057334

반응식

HRID 2057334 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]([C@H:13]2[CH2:18][CH2:17][C@H:16]([OH:19])[CH2:15][CH2:14]2)[CH3:12])(=[O:10])=[O:9])=[CH:4][CH:3]=1.Cl.[CH2:21]([N:23]([CH2:27][CH3:28])[CH2:24][CH2:25]Cl)[CH3:22].[OH-].[Na+]>C1(C)C=CC=CC=1.[N+](CCCC)(CCCC)(CCCC)CCCC.[O-]S(O)(=O)=O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]([C@H:13]2[CH2:18][CH2:17][C@H:16]([O:19][CH2:22][CH2:21][N:23]([CH2:27][CH3:28])[CH2:24][CH3:25])[CH2:15][CH2:14]2)[CH3:12])(=[O:9])=[O:10])=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 133631-Chloro-2-(diethylamine)ethane hydrochlorideHCID 14798Sodium HydroxideHCID 178484844HCID 178484844, 화합물

생성물 1

HCID 178464092HCID 178464092, 화합물수율 84.9%

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 1140Toluene용매

실험 절차

To 350 mg (1 mmol) trans-4-Bromo-N-(4-hydroxy-cyclohexyl)-N-methyl-benzenesulfonamide in 6 ml toluene was added 344 mg (2.0 mmol) 2-diethylamino-ethylchlorid.hydrochloride and a catalytic amount of Bu4NHSO4 followed by 4 ml 50% NaOH. The mixture was stirred at RT over night, the phases were separated and the organic phase dried over Na2SO4. Column chromatography on silica gel with CH2Cl2/MeOH 15:1 yielded 380 mg (84%) trans-4-Bromo-N-[4-(2-diethylamino-ethoxy)-cyclohexyl]-N-methyl-benzenesulfonamide as light yellow oil, MS: 447 (MH+, 1Br).

후처리

  1. customthe phases were separated
  2. dry with materialthe organic phase dried over Na2SO4

출처 및 근거

ORD 기록
ord-b42e8bf3c8d34bb68b887b895d37e0d5
출처 데이터셋
uspto-grants-2008_02
특허 번호
US07335687B2

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