氨 → 4-Methyl-5-nitrosaccharin

HRID 808

反应方程式

HRID 808 反应方程式
[NH3:1].O.C[O:4][C:5]([C:7]1[C:12]([CH3:13])=[C:11]([N+:14]([O-:16])=[O:15])[CH:10]=[CH:9][C:8]=1[S:17](Cl)(=[O:19])=[O:18])=O>O1CCCC1>[CH3:13][C:12]1[C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=[C:8]2[C:7]=1[C:5](=[O:4])[NH:1][S:17]2(=[O:19])=[O:18]

参与物

5

反应物 3

HCID 222氨HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 153345332-Methoxycarbonyl-3-methyl-4-nitrobenzenesulfonyl chloride

产物 1

HCID 153345344-Methyl-5-nitrosaccharin

试剂、催化剂与溶剂 1

HCID 8028四氢呋喃溶剂

反应条件

温度
25 °C

实验过程

104 ml of 25% ammonia solution are initially taken, 100 ml of water are added and a solution of 48.7 g (0.166 mol) of 2-methoxycarbonyl-3-methyl-4-nitrobenzenesulfonyl chloride in 70 ml of tetrahydrofuran is then added dropwise at 10° C. After stirring at 25° C. for three hours, the mixture is concentrated on a rotary evaporator to remove water and THF. The residue which remains is stirred with ethyl acetate, filtered off with suction and washed with ethyl acetate. After drying under reduced pressure, 34 g (0.131 mol)=79% of theory of a white solid of m.p.: 312° C. (dec.) are obtained.

后处理

  1. concentrationthe mixture is concentrated on a rotary evaporator
  2. customto remove water and THF
  3. stirringThe residue which remains is stirred with ethyl acetate
  4. filtrationfiltered off with suction
  5. washwashed with ethyl acetate
  6. customAfter drying under reduced pressure, 34 g (0.131 mol)=79% of theory of a white solid of m.p.: 312° C. (dec.)
  7. customare obtained

来源与证据

ORD记录
ord-9750ebabdd9f4e72aa5a98408ce4247f
来源数据集
uspto-grants-1998_03
专利号
US05723415

关联笔记

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