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

HRID 2396135
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HRID 2396135 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
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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 kith 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 2M sodium carbonate solution. After washing the ethyl acetate layer kith water and drying kithsodium sulfate the solvent is evaporated. Recrystallization from toluene gives 27,2 g (73%) of the product having m.p. 135°-9° C.

후처리

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

출처 및 근거

ORD 기록
ord-1e00268a0a5e46968d0ae35200562364
출처 데이터셋
uspto-grants-1996_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05491173

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