Water → HCID 18706355, 화합물

HRID 1422219노트

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HRID 1422219 반응식
[N:1]([CH2:4][C:5]1[CH:14]=[C:13]([Br:15])[CH:12]=[C:11]2[C:6]=1[NH:7][CH:8]([O:18][CH3:19])[CH:9]([O:16][CH3:17])[NH:10]2)=[N+]=[N-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O>O1CCCC1>[NH2:1][CH2:4][C:5]1[CH:14]=[C:13]([Br:15])[CH:12]=[C:11]2[C:6]=1[NH:7][CH:8]([O:18][CH3:19])[CH:9]([O:16][CH3:17])[NH:10]2

참가 물질

5

반응물 3

HCID 962WaterHCID 11776TriphenylphosphineHCID 18706342HCID 18706342, 화합물

생성물 1

HCID 18706355HCID 18706355, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
20 °C

실험 절차

4.47 g (13.8 mmol) of 5-azidomethyl-7-bromo-2,3-dimethoxy-1,2,3,4-tetrahydroquinoxaline are dissolved in 35 ml of tetrahydrofuran, and 3.98 g (1.1 equiv.) of triphenylphosphine are added. The mixture is stirred at 20° C. for 4 hours. 746 mg of water are added and the mixture is stirred for a further three hours. The solid is filtered off and the filtrate is extracted with ethyl acetate and sodium carbonate solution. The organic phases are combined, washed with brine, dried over magnesium sulfate and concentrated by evaporation. The residue is chromatographed on silica gel with ethyl acetate/petroleum ether (1:1).

후처리

  1. stirringthe mixture is stirred for a further three hours
  2. filtrationThe solid is filtered off
  3. extractionthe filtrate is extracted with ethyl acetate and sodium carbonate solution
  4. washwashed with brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated by evaporation
  7. customThe residue is chromatographed on silica gel with ethyl acetate/petroleum ether (1:1)

출처 및 근거

ORD 기록
ord-59dc08a3d9ec4189a9411ef1c988f31b
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06080743

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