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Sodium Bicarbonate → HCID 58028448, 화합물

HRID 1399416
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HRID 1399416 반응식
[Na+].[CH2:2]([C:8]1[S:12][C:11](OB(O)[O-])=[CH:10][CH:9]=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].Br[C:18]1[CH:23]=[CH:22][C:21]([C:24]2[CH:29]=[CH:28][C:27]([CH2:30][CH2:31][CH2:32][CH2:33][CH3:34])=[CH:26][CH:25]=2)=[C:20]([F:35])[CH:19]=1.C(=O)([O-])O.[Na+]>C1COCC1.O.CC(OC)(C)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[F:35][C:20]1[CH:19]=[C:18]([C:11]2[S:12][C:8]([CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7])=[CH:9][CH:10]=2)[CH:23]=[CH:22][C:21]=1[C:24]1[CH:29]=[CH:28][C:27]([CH2:30][CH2:31][CH2:32][CH2:33][CH3:34])=[CH:26][CH:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 516892Sodium BicarbonateHCID 227175154-Bromo-2-fluoro-4'-pentyl-1,1'-biphenylHCID 131730280HCID 131730280, 화합물

생성물 1

HCID 58028448HCID 58028448, 화합물

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매
HCID 15413
tert-Butyl methyl ether
용매
HCID 21881883Oxolane--water (1/1)용매

실험 절차

A mixture of 3.30 g (13.1 mmol) of 5-hexylthiophen-2-ylhydroxyboronic acid sodium salt, 4.20 g (13.1 mmol) of 4-bromo-2-fluoro-4′-pentylbiphenyl, 2.2 g (26.2 mmol) of sodium hydrogencarbonate and 0.70 g (0.61 mmol) of tetrakis(triphenylphosphine)palladium(0) in THF/water (1:1) is heated under reflux for 6 h. The mixture is diluted with MTBE, and the organic phase is separated off. The aqueous phase is extracted with MTBE. The combined organic phases are washed with sat. sodium chloride solution and dried using sodium sulfate. The solution is evaporated to dryness, and the residue is purified by column chromatography (SiO2, n-heptane). The further purification is carried out by recrystallisation from methanol/pentane (5:1), giving 2-(2-fluoro-4′-pentylbiphenyl-4-yl)-5-hexylthiophene as a colourless solid having an m.p. of 44° C.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 6 h
  3. customthe organic phase is separated off
  4. extractionThe aqueous phase is extracted with MTBE
  5. washThe combined organic phases are washed with sat. sodium chloride solution
  6. customdried
  7. customThe solution is evaporated to dryness
  8. customthe residue is purified by column chromatography (SiO2, n-heptane)
  9. customThe further purification
  10. customis carried out by recrystallisation from methanol/pentane (5:1)

출처 및 근거

ORD 기록
ord-8c4d01e596614ee5ab4d9234423106b9
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08906261B2

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