Water → HCID 23123945, 화합물

HRID 350845노트

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HRID 350845 반응식
[CH2:1]1[CH2:17][O:16][C:3]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)([CH2:4][CH2:5][CH2:6][N:7]=[N+]=[N-])[O:2]1.O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(=O)([O-])O.[Na+]>O1CCCC1>[CH2:17]1[CH2:1][O:2][C:3]([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)([CH2:4][CH2:5][CH2:6][NH2:7])[O:16]1

참가 물질

6

반응물 4

HCID 962WaterHCID 11776TriphenylphosphineHCID 516892Sodium BicarbonateHCID 231239164,4-Ethylenedioxy-4-phenylbutylazide

생성물 1

HCID 23123945HCID 23123945, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

4,4-Ethylenedioxy-4-phenylbutylazide (130.0 mg, 0.56 mmol) was dissolved in tetrahydrofuran (5 ml), and thereto were added water (0.01 ml, 0.56 mmol) and triphenylphosphine (146.2 mg, 0.56 mmol) in a tetrahydrofuran solution (2 ml) in sequential order at the same temperature, and thereafter, the solution was stirred at room temperature for 24 hours. The reaction solution was added to a saturated aqueous sodium hydrogencarbonate solution and then extracted by chloroform, to obtain an organic layer. The extracted organic was washed with brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resultant substance was purified by silica gel column chromatography (chloroform/methanol=10/1), whereby the target compound was obtained as a colorless oil (61.8 mg, 56.4% for 2 steps).

후처리

  1. extractionextracted by chloroform
  2. customto obtain an organic layer
  3. washThe extracted organic was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resultant substance was purified by silica gel column chromatography (chloroform/methanol=10/1), whereby the target compound
  7. customwas obtained as a colorless oil (61.8 mg, 56.4% for 2 steps)

출처 및 근거

ORD 기록
ord-714385c1810d4cc9bf9d7a9582723540
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07183295B2

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