Water → HCID 18706355、化合物

HRID 1422219ノート

反応式

HRID 1422219 の反応式
[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

参加物

5

反応物 3

HCID 962WaterHCID 11776TriphenylphosphineHCID 18706342HCID 18706342、化合物

生成物 1

HCID 18706355HCID 18706355、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
20 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-59dc08a3d9ec4189a9411ef1c988f31b
出典データセット
uspto-grants-2000_06
特許番号
US06080743

反応ノート

読み込み中…