Hexamethyldisilazane → Ethyl 2-sulfamoylacetate

HRID 648189

反応式

HRID 648189 の反応式
[CH2:1]([O:3][C:4]([CH2:6][S:7](Cl)(=[O:9])=[O:8])=[O:5])[CH3:2].C[Si](C)(C)[NH:13][Si](C)(C)C>C(Cl)Cl>[CH2:1]([O:3][C:4]([CH2:6][S:7]([NH2:13])(=[O:9])=[O:8])=[O:5])[CH3:2]

参加物

4

反応物 2

HCID 13838HexamethyldisilazaneHCID 12225100Ethyl (chlorosulfonyl)acetate

生成物 1

HCID 12225113Ethyl 2-sulfamoylacetate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 54.6 g (0.29 mole) ethoxy carbonyl methanesulfonyl chloride in 250 ml methylene chloride is stirred at 0° under a nitrogen atmosphere while 46.8 g (0.29 mole) hexamethyldisilazane is added dropwise. The resulting cloudy solution is allowed to warm to 25° over one hour and then evaporated in vacuo to an oil which crystallizes: yield of the title product is 48.4 g (100%), mp 63°-67°; lit.1 mp 67°-68°, lit2 mp 66°-68°.

後処理

  1. additionis added dropwise
  2. temperatureto warm to 25° over one hour
  3. customevaporated in vacuo to an oil which
  4. customcrystallizes

出典と根拠

ORDレコード
ord-ccbb9e39cb8f49eaa411d4555b4ce37c
出典データセット
uspto-grants-1983_10
特許番号
US04411899

関連ノート

読み込み中…