Tetrahydrofuran → HCID 59511923, 화합물

HRID 1157945노트

반응식

HRID 1157945 반응식
[N:1]([CH2:4][C:5]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:6]=1[Br:14])=[N+]=[N-].C1COCC1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O>[Br:14][C:6]1[CH:7]=[CH:8][C:9]([N+:11]([O-:13])=[O:12])=[CH:10][C:5]=1[CH2:4][NH2:1]

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 11776TriphenylphosphineHCID 59511835Benzene, 2-(azidomethyl)-1-bromo-4-nitro-

생성물 1

HCID 59511923HCID 59511923, 화합물수율 95.5%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

To a mixture of 2-azidomethyl-1-bromo-4-nitrobenzene (6.57 g) and THF (50 mL) there was added triphenylphosphine (7.05 g) at 0° C. under a nitrogen atmosphere. The mixture was stirred at 0° C. for 1 hour and then at room temperature for 2 hours, after which water (10 mL) was added and the mixture was heated to reflux for 15 hours. The solvent in the mixture was distilled off under reduced pressure and the residue was purified by NH silica gel column chromatography (ethyl acetate-heptane mixture) to obtain the target compound (5.64 g) as a colorless solid.

후처리

  1. waitat room temperature for 2 hours
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 15 hours
  4. distillationThe solvent in the mixture was distilled off under reduced pressure
  5. customthe residue was purified by NH silica gel column chromatography (ethyl acetate-heptane mixture)

출처 및 근거

ORD 기록
ord-f4a93e35107043909174e19546bd1416
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07807690B2

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