Sodium Carbonate → 1-Phenyl-1-cyclohexyl-3-(2-tritylaminoethyl)amino-1-propanol

HRID 1074159노트

반응식

HRID 1074159 반응식
[C:1]([NH:20][CH2:21][CH2:22][NH2:23])([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[C:30]1([C:36]([CH:41]2[CH2:46][CH2:45][CH2:44][CH2:43][CH2:42]2)([OH:40])[CH2:37][CH2:38]Cl)[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1>C(O)CCC.O>[C:30]1([C:36]([CH:41]2[CH2:46][CH2:45][CH2:44][CH2:43][CH2:42]2)([OH:40])[CH2:37][CH2:38][NH:23][CH2:22][CH2:21][NH:20][C:1]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 2794294N-tritylethylenediamineHCID 138411961-Phenyl-1-cyclohexyl-3-chloro-1-propanol

생성물 1

HCID 221558931-Phenyl-1-cyclohexyl-3-(2-tritylaminoethyl)amino-1-propanol수율 61.7%

시약·촉매·용매 2

HCID 2631-Butanol용매2회HCID 962Water용매

실험 절차

To a mixture of N-tritylethylenediamin (3.66 g) and sodium carbonate (9.2 g) in n-butanol (20 ml), a solution of 1-phenyl-1-cyclohexyl-3-chloro-1-propanol (3 g) in butanol (10 ml) was added. The mixture was refluxed overnight, then cooled, diluted with water and extracted with ethyl acetate. The solvent was dried and evaporated. The residue was purified by column chromatography (methylene chloride, methanol, ammonia 99:1:0.1) to afford 3.8 g of 1-phenyl-1-cyclohexyl-3-(2-tritylaminoethyl)amino-1-propanol. M.p. 198° C.

후처리

  1. temperatureThe mixture was refluxed overnight
  2. temperaturecooled
  3. extractionextracted with ethyl acetate
  4. customThe solvent was dried
  5. customevaporated
  6. customThe residue was purified by column chromatography (methylene chloride, methanol, ammonia 99:1:0.1)

출처 및 근거

ORD 기록
ord-f16a00da4a854242a00f90236b9c3b57
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04973592

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