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Dimethyl Sulfoxide → HCID 20540358, 화합물

HRID 1065466
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HRID 1065466 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH2:8][CH:9]([NH:11][CH2:12][CH2:13][CH:14]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH3:10])[CH:5]=[CH:6][CH:7]=1.CS(C)=O.[OH-].[Na+].[Cl:33][C:34]1[CH:41]=[CH:40][C:37]([CH2:38]Cl)=[CH:36][CH:35]=1>O>[ClH:33].[Cl:33][C:34]1[CH:41]=[CH:40][C:37]([CH2:38][O:1][C:2]2[CH:3]=[C:4]([CH2:8][CH:9]([NH:11][CH2:12][CH2:13][CH:14]([C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)[CH3:10])[CH:5]=[CH:6][CH:7]=2)=[CH:36][CH:35]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 77231-Chloro-4-(chloromethyl)benzeneHCID 14798Sodium HydroxideHCID 130652773-[2-[(3,3-Diphenylpropyl)amino]propyl]phenol

생성물 1

HCID 20540358HCID 20540358, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

The mixture of 17.3 g of 1-(3-hydroxyphenyl)-2-(3,3-diphenylpropylamino)-propane, 100 ml of dimethylsulfoxide and 5 ml of 10 N-aqueous sodium hydroxide is stirred at room temperature for 1/2 hour, combined with 8.05 g of 4-chlorobenzyl chloride and stirred 16 hours longer. It is poured into water, extracted with ethyl acetate, the extract washed with saturated aqueous sodium chloride, dried and evaporated. The residue is taken up in diethyl ether, the solution acidified with isopropanolic hydrogen chloride, the precipitate collected and washed with diethyl ether, to yield the 1-[3-(4-chlorobenzyloxy)-phenyl]-2-(3,3-diphenylpropylamino)-propane hydrochloride melting at 184°-189°.

후처리

  1. stirringstirred 16 hours longer
  2. extractionextracted with ethyl acetate
  3. washthe extract washed with saturated aqueous sodium chloride
  4. customdried
  5. customevaporated
  6. customthe precipitate collected
  7. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-5757b4918a3d42b59512b9095102c85b
출처 데이터셋
uspto-grants-1982_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04329367

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