Chlorosulfonyl isocyanate → HCID 14722020、化合物

HRID 326974ノート

反応式

HRID 326974 の反応式
Cl[S:2]([N:5]=[C:6]=[O:7])(=[O:4])=[O:3].[CH3:8][O:9][C:10]1[CH:19]=[CH:18][CH:17]=[C:12]([C:13]([O:15][CH3:16])=[O:14])[C:11]=1[OH:20]>C1(C)C(C)=CC=CC=1>[CH3:16][O:15][C:13](=[O:14])[C:12]1[CH:17]=[CH:18][CH:19]=[C:10]([O:9][CH3:8])[C:11]=1[O:20][S:2]([N:5]=[C:6]=[O:7])(=[O:4])=[O:3]

参加物

4

反応物 2

HCID 70918Chlorosulfonyl isocyanateHCID 80651Methyl 3-methoxysalicylate

生成物 1

HCID 14722020HCID 14722020、化合物

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
140 °C

実験手順

3.4 g (0.024 mol) of chlorosulfonyl isocyanate are added dropwise to a solution of 3.6 g (0.02 mol) of methyl 3-methoxy-salicylate in 20 ml of xylene at 25° C. When the dropwise addition has ended, the temperature is slowly increased to 140° C. and the mixture is heated under reflux for 2.5 hours. It is cooled and the solvent and excess chlorosulfonyl isocyanate are removed on a rotary evaporator. The yellow oil which remains (5.4 g=1004 of theory) is used without further purification.

後処理

  1. additionWhen the dropwise addition
  2. temperaturethe mixture is heated
  3. temperatureunder reflux for 2.5 hours
  4. temperatureIt is cooled
  5. customthe solvent and excess chlorosulfonyl isocyanate are removed on a rotary evaporator
  6. customis used without further purification

出典と根拠

ORDレコード
ord-acdd9fd9f7d44198b26daaec0a1a2fd4
出典データセット
uspto-grants-1993_12
特許番号
US05272129

反応ノート

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