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Triphenylphosphine → HCID 23136285, 화합물

HRID 1678589
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HRID 1678589 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH:5]=[CH:6][C:7]=1[OH:8].[O:16]([C:23]1[CH:28]=[CH:27][C:26]([CH2:29]O)=[CH:25][CH:24]=1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>O1CCCC1.C1(C)C=CC=CC=1.O>[F:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH:5]=[CH:6][C:7]=1[O:8][CH2:29][C:26]1[CH:27]=[CH:28][C:23]([O:16][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)=[CH:24][CH:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 826195(4-Phenoxyphenyl)methanolHCID 3023769Ethyl 3-(3-fluoro-4-hydroxyphenyl)propionate

생성물 1

HCID 23136285HCID 23136285, 화합물수율 71%

시약·촉매·용매 3

HCID 962
Water
용매
HCID 1140Toluene용매
HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of ice-cooled ethyl 3-(3-fluoro-4-hydroxyphenyl)propanoate (0.19 g, 0.88 mmol), (4-phenoxyphenyl)methanol (0.12 g, 0.58 mmol) and triphenylphosphine (0.23 g, 0.88 mmol) in tetrahydrofuran (5 mL) was added dropwise diethyl azodicarboxylate (a 40% solution in toluene, 0.40 mL, 0.88 mmol), and the mixture was stirred at room temperature for 4 hours. To the reaction solution was added water, and the reaction mixture was extracted with ethyl acetate. The extract was washed with water, and then concentrated under reduced pressure. The residue was purified with silica gel column chromatography (hexane/ethyl acetate=8:2) to give the title compound (0.16 g, yield 71%) as an oily matter.

후처리

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washThe extract was washed with water
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified with silica gel column chromatography (hexane/ethyl acetate=8:2)

출처 및 근거

ORD 기록
ord-c85ee14e54504e02b5691f8d4725a689
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08008525B2

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