Triphenylphosphine → HCID 117620688, 화합물

HRID 626319노트

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HRID 626319 반응식
N(C(OCCOC)=O)=NC(OCCOC)=O.[CH3:17][C:18]1[CH:23]=[C:22]([N+:24]([O-:26])=[O:25])[C:21]([CH3:27])=[CH:20][C:19]=1[OH:28].[Br:29][C:30]1([Br:35])[CH2:32][CH:31]1[CH2:33]O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(=O)(O)[O-].[Na+]>C1(C)C=CC=CC=1>[Br:29][C:30]1([Br:35])[CH2:32][CH:31]1[CH2:33][O:28][C:19]1[CH:20]=[C:21]([CH3:27])[C:22]([N+:24]([O-:26])=[O:25])=[CH:23][C:18]=1[CH3:17]

참가 물질

7

반응물 5

HCID 11776TriphenylphosphineHCID 2821102,5-Dimethyl-4-nitrophenolHCID 516892Sodium BicarbonateHCID 108897082,2-DibromocyclopropanemethanolHCID 533844152-methoxyethyl N-(2-methoxyethoxycarbonylimino)carbamate

생성물 1

HCID 117620688HCID 117620688, 화합물수율 36%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

0.85 g of Bis(2-methoxyethyl) azodicarboxylate was added to a mixture of 0.47 g of 2,5-dimethyl-4-nitrophenol, 0.64 g of (2,2-dibromocyclopropyl)methanol (manufactured according to a reference document (R. Huwyler, A. Al-Dulayymi, M. Neuenschwander, Helv. Chim. Acta 1999, 82, 2336)), 0.87 g of triphenylphosphine and 30 mL of toluene at 0° C., and the mixture was stirred at 80° C. for 5 hours. After cooling, a saturated aqueous sodium bicarbonate solution was added, and the mixture was extracted with ethyl acetate, and then the organic layer was washed with water and saturated salt water and dried over anhydrous magnesium sulfate. The resulting residue was subjected to silica gel column chromatography to obtain 0.38 g of 1-[(2,2-dibromo-cyclopropyl)methoxy]-2,5-dimethyl-4-nitrobenzene.

후처리

  1. temperatureAfter cooling
  2. extractionthe mixture was extracted with ethyl acetate
  3. washthe organic layer was washed with water and saturated salt water
  4. dry with materialdried over anhydrous magnesium sulfate

출처 및 근거

ORD 기록
ord-9ffa8bbfa9a24193ab73d42a9ed154b9
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309191B2

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