1-Ethenyl-4-nitrobenzene → HCID 178502925, 화합물

HRID 1252550

반응식

HRID 1252550 반응식
[PH2](O)=O.C(OC)(OC)OC.[PH2:11]([O:13][CH3:14])=[O:12].[N+:15]([C:18]1[CH:25]=[CH:24][C:21]([CH:22]=[CH2:23])=[CH:20][CH:19]=1)([O-:17])=[O:16].C(N(C(C)C)CC)(C)C.C(=O)(O)[O-].[Na+]>CO.O>[CH3:14][O:13][PH:11]([CH2:23][CH2:22][C:21]1[CH:20]=[CH:19][C:18]([N+:15]([O-:17])=[O:16])=[CH:25][CH:24]=1)=[O:12]

참가 물질

9

반응물 6

HCID 74811-Ethenyl-4-nitrobenzeneHCID 9005Trimethyl orthoformateHCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 4124402Phosphinic AcidHCID 178502919HCID 178502919, 화합물2회

생성물 1

HCID 178502925HCID 178502925, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
20 °C

실험 절차

0.665 g of crystalline hypophosphorous acid was treated under nitrogen with 1.73 g of trimethyl orthoformate and the mixture was stirred at 20° C. for 2 hours. The resulting solution of crude methyl hypophosphite was added dropwise at 0° C. to a solution of 1 g of 4-nitrostyrene and 0.43 g of diisopropylethylamine in 5 ml of methanol. After 65 hours at 20° C. the same amount of methyl hypophosphite was again added and the mixture was stirred at 20° C. for a further 24 hours. The mixture was diluted with 30 ml of water and the pH was adjusted to 7 with aqueous sodium bicarbonate solution. After extraction with dichloromethane and chromatography on silica gel using 10% methanol in ethyl acetate for the elution there was obtained 0.5 g of 1-[2-(methoxyphosphinyl)ethyl]-4-nitrobenzene in the form of a yellow liquid.

후처리

  1. stirringthe mixture was stirred at 20° C. for a further 24 hours
  2. extractionAfter extraction with dichloromethane and chromatography on silica gel using 10% methanol in ethyl acetate
  3. washfor the elution there

출처 및 근거

ORD 기록
ord-f4c21074e7fa4b37a69f58637e826285
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04743687

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