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4-Hydroxybiphenyl → HCID 803546, 화합물

HRID 1250463
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HRID 1250463 반응식
O[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.Cl[CH2:15][CH2:16][N:17]1[CH2:21][CH2:20][CH2:19][CH2:18]1.C(=O)([O-])[O-:23].[K+].[K+]>CN(C)C=O>[C:5]1([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:4]([O:23][CH2:15][CH2:16][N:17]2[CH2:21][CH2:20][CH2:19][CH2:18]2)=[CH:3][CH:2]=[CH:7][CH:6]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 71034-HydroxybiphenylHCID 11430Potassium CarbonateHCID 816691-(2-Chloroethyl)pyrrolidine

생성물 1

HCID 803546HCID 803546, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

1.76 mol of 4-hydroxybiphenyl, 2.29 mol of 1-(2-chloroethyl)pyrrolidine and 5.3 mol of potassium carbonate are placed in 2.5 liters of dimethylformamide. The whole is heated at 50° C. ovemright. After cooling, the solid is filtered off and the solvent is removed by evaporation. The residue is taken up in ethyl acetate. After washing of the organic phase drying and evaporation, a residue is obtained which is purified by chromatography over silica using an ethyl acetate/ethanol mixture (80/20) as eluant. The expected product is obtained after crystallisation of the residual oil.

후처리

  1. temperatureAfter cooling
  2. filtrationthe solid is filtered off
  3. customthe solvent is removed by evaporation
  4. washAfter washing of the organic phase
  5. customdrying
  6. customevaporation
  7. customa residue is obtained which
  8. customis purified by chromatography over silica using an ethyl acetate/ethanol mixture (80/20) as eluant

출처 및 근거

ORD 기록
ord-f8639d41aa56444a9d4d80a32c962af0
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06339092B1

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