Tetrahydrofuran → HCID 59511923、化合物

HRID 1157945ノート

反応式

HRID 1157945 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 59511923HCID 59511923、化合物収率 95.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-f4a93e35107043909174e19546bd1416
出典データセット
uspto-grants-2010_10
特許番号
US07807690B2

反応ノート

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