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(Diethylamino)sulfur trifluoride → HCID 86646156, 화합물

HRID 551690
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HRID 551690 반응식
O[CH2:2][CH2:3][CH:4]([CH2:12][CH:13]=[CH2:14])/[CH:5]=[CH:6]/[C:7]([O:9][CH2:10][CH3:11])=[O:8].CCN(S(F)(F)[F:21])CC.C(=O)(O)[O-].[Na+]>O1CCCC1>[F:21][CH2:2][CH2:3][CH:4]([CH2:12][CH:13]=[CH2:14])/[CH:5]=[CH:6]/[C:7]([O:9][CH2:10][CH3:11])=[O:8]
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참가 물질

5

반응물 3

HCID 123472(Diethylamino)sulfur trifluorideHCID 516892Sodium BicarbonateHCID 86646155HCID 86646155, 화합물

생성물 1

HCID 86646156HCID 86646156, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Ethyl(E)-4-(2-hydroxyethyl)-hepta-2,6-dienoate (5 g, 27.1 mmol) was dissolved in tetrahydrofuran (40 mL). To the solution, DAST (4.8 g, 29.8 mmol) was added under ice cooling, and the mixture was stirred for 1 hour. The reaction solution was poured to a saturated aqueous solution of sodium bicarbonate, followed by extraction with ethyl acetate. The ethyl acetate layer was washed with saturated saline, then dried, and then concentrated. The residue was purified by silica gel column chromatography (200 g) to obtain the compound of interest as an oil substance (2.2 g, 44%).

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe ethyl acetate layer was washed with saturated saline
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography (200 g)
  6. customto obtain the compound of interest as an oil substance (2.2 g, 44%)

출처 및 근거

ORD 기록
ord-1842d5e3a2244ce7a6e4fa78749afee2
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07947738B2

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