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Methylamine → 1,2-diphenyl-1-[4-[2-(N-methylamino)ethoxy]phenyl]-1-buten-4-ol

HRID 982443
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HRID 982443 반응식
[C:1]1(/[C:7](/[C:18]2[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26]Br)=[CH:20][CH:19]=2)=[C:8](/[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)\[CH2:9][CH2:10][OH:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:28][NH2:29]>C(O)C>[C:1]1([C:7]([C:18]2[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26][NH:29][CH3:28])=[CH:20][CH:19]=2)=[C:8]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:9][CH2:10][OH:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 69544510Z-1,2-diphenyl-1-[4-(bromoethoxy)phenyl]-1-buten-4-ol

생성물 1

HCID 542527341,2-diphenyl-1-[4-[2-(N-methylamino)ethoxy]phenyl]-1-buten-4-ol수율 73%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

42.3 g of (Z)-1,2-diphenyl-1-[4-(2-bromoethoxy)phenyl]-1-buten-4-ol is stirred over 500 ml of 33% methylamine in ethanol for 10 h at 100° C. in autoclave. The solvent is evaporated and the evaporation residue is dissolved in ethyl acetate in the presence of 2 M sodium carbonate solution. After washing the ethyl acetate layer with water and drying with sodium sulfate the solvent is evaporated. Recrystallization from toluene gives 27.2 g (73%) of the product having m.p. 134°-9° C.

후처리

  1. customThe solvent is evaporated
  2. dissolutionthe evaporation residue is dissolved in ethyl acetate in the presence of 2 M sodium carbonate solution
  3. washAfter washing the ethyl acetate layer with water
  4. dry with materialdrying with sodium sulfate the solvent
  5. customis evaporated
  6. customRecrystallization from toluene

출처 및 근거

ORD 기록
ord-303fe089d18746bca68f7deeb58af049
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04996225

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