4-Nitrobenzenesulfonyl chloride → HCID 874568、化合物

HRID 624231ノート

反応式

HRID 624231 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10](Cl)(=[O:12])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].C(N(C(C)C)CC)(C)C.[CH3:23][CH:24]([CH3:28])[CH2:25][CH2:26][NH2:27]>ClCCl.C(=O)(O)[O-].[Na+]>[CH2:26]([NH:27][S:10]([C:7]1[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1)(=[O:12])=[O:11])[CH2:25][CH:24]([CH3:28])[CH3:23]

参加物

6

反応物 3

HCID 74044-Nitrobenzenesulfonyl chlorideHCID 7894IsoamylamineHCID 81531Diisopropylethylamine

生成物 1

HCID 874568HCID 874568、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 516892Sodium Bicarbonate溶媒

反応条件

温度
0 °C

実験手順

4-Nitrobenzene-1-sulfonyl chloride (1.5 g, 6.57 mmol) was dissolved in dichloromethane (30 ml) and cooled to 0° C. followed by addition of diisopropylethylamine (2.293 ml, 13.13 mmol). 3-Methylbutan-1-amine (0.926 ml, 7.88 mmol) was dissolved in 5 ml dichloromethane and added via syringe. After the addition, the mixture was allowed to warm to room temperature for 3 hours. The solution was diluted with aqueous sodium bicarbonate and extracted twice with dichloromethane. The organics were combined, dried over magnesium sulfate, filtered and concentrated. Chromatography provided the title compound.

後処理

  1. additionadded via syringe
  2. additionAfter the addition
  3. temperatureto warm to room temperature for 3 hours
  4. extractionextracted twice with dichloromethane
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-d0c461296de4417fb3d1e87938df67cf
出典データセット
uspto-grants-2016_04
特許番号
US09302989B2

反応ノート

読み込み中…