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Triethylamine → HCID 86647488, 화합물

HRID 1808303
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HRID 1808303 반응식
[CH2:1]([O:5][C:6]1[CH:7]=[C:8]([CH:11]=[CH:12][C:13]=1[OH:14])[CH:9]=O)[CH2:2][CH2:3][CH3:4].[Cl-].[CH3:16][O:17][CH:18]([P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[C:19]([O:21][CH3:22])=[O:20].C(N(CC)CC)C>O1CCCC1>[CH2:1]([O:5][C:6]1[CH:7]=[C:8](/[CH:9]=[C:18](\[O:17][CH3:16])/[C:19]([O:21][CH3:22])=[O:20])[CH:11]=[CH:12][C:13]=1[OH:14])[CH2:2][CH2:3][CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 11429511HCID 11429511, 화합물HCID 19261375HCID 19261375, 화합물

생성물 1

HCID 86647488HCID 86647488, 화합물수율 92%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
40 °C

실험 절차

4.0 g (20.6 mmol) of 3-butoxy-4-hydroxybenzaldehyde and 13.25 g (30.9 mmol) of (methoxy(methoxycarbonyl)methyl)triphenylphosphonium chloride are suspended in 40 ml of tetrahydrofuran. 6 ml (42 mmol) of triethylamine are added and then the reaction medium is stirred at 40° C. for 16 hours. The reaction medium is filtered and then the solvents are evaporated. 50 ml of diethyl ether are added and the mixture is stirred at ambient temperature for 10 minutes and then filtered. After evaporation of the solvents, the residue is taken up in a heptane/ethyl acetate 8/2 mixture and then filtered through a silica patch (2 cm). 5.3 g of methyl (Z)-3-(3-butoxy-4-hydroxyphenyl)-2-methoxyacrylate are obtained after evaporation of the solvents.

후처리

  1. filtrationThe reaction medium is filtered
  2. customthe solvents are evaporated
  3. addition50 ml of diethyl ether are added
  4. stirringthe mixture is stirred at ambient temperature for 10 minutes
  5. filtrationfiltered
  6. customAfter evaporation of the solvents
  7. filtrationfiltered through a silica patch (2 cm)

출처 및 근거

ORD 기록
ord-060def5dc783482cbe836a79af49b696
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08357819B2

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