Isopropylamine → N,N'-diisopropylsulfamide

HRID 2413118ノート

反応式

HRID 2413118 の反応式
[CH:1]([NH2:4])([CH3:3])[CH3:2].C([N:7]([CH2:10][CH3:11])CC)C.[CH3:12][Si](C)(C)Cl.[S:17](Cl)(Cl)(=[O:19])=[O:18]>C1COCC1>[CH:1]([NH:4][S:17]([NH:7][CH:10]([CH3:11])[CH3:12])(=[O:19])=[O:18])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 6363IsopropylamineHCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 24648Sulfuryl chloride

生成物 1

HCID 2818101N,N'-diisopropylsulfamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

29.5 parts of isopropylamine and 55.6 parts of triethylamine were introduced into 320 parts of THF. 60 parts of trimethylchlorosilane were added a little at a time at from 0° to -5° C. under nitrogen and the mixture was stirred at room temperature for 30 minutes and at 60° C. for 1 hour and then cooled to -10° C. 33.8 parts of sulfuryl chloride were added a little at a time and the mixture was allowed to warm to room temperature and was then stirred for 2 hours. The trimethylchlorosilane and the solvent were distilled off and the residue was washed with ice-water. 30.5 parts of N,N'-diisopropylsulfamide of melting point 98°-101° C. (starting substance) were obtained.

後処理

  1. temperaturecooled to -10° C
  2. temperatureto warm to room temperature
  3. stirringwas then stirred for 2 hours
  4. distillationThe trimethylchlorosilane and the solvent were distilled off
  5. washthe residue was washed with ice-water

出典と根拠

ORDレコード
ord-537efb687c614dd997e9a19df243bc62
出典データセット
uspto-grants-1985_01
特許番号
US04496563

反応ノート

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