Sodium sulfide nonahydrate → 2-(2,3-Diamino-5-nitrophenyl)ethanol

HRID 4760

反应方程式

HRID 4760 反应方程式
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][C:5]([N+:11]([O-:13])=[O:12])=[CH:4][C:3]=1[CH2:14][CH2:15][OH:16].O.O.O.O.O.O.O.O.O.[S-2].[Na+].[Na+].[S]>C(O)(C)C.O>[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][C:5]([N+:11]([O-:13])=[O:12])=[CH:4][C:3]=1[CH2:14][CH2:15][OH:16]

参与物

6

反应物 3

HCID 73972Sodium sulfide nonahydrateHCID 5362487不溶性硫黄HCID 198363402-(2-Amino-3,5-dinitrophenyl)ethanol

产物 1

HCID 198363412-(2,3-Diamino-5-nitrophenyl)ethanol

试剂、催化剂与溶剂 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂2 次HCID 3776异丙醇溶剂

实验过程

To a suspension of 0.119 mole (27 g) of 2-(2-amino-3,5-dinitrophenyl)ethanol obtained in Example 1 in 67.5 ml of isopropanol to which an equal volume of water has been added, a solutionof 38.4 g of sodium sulphide nonahydrate and 5.4 g of sulphur in 10 ml of water is added dropwise at 60°-65° C. Heating is maintained for 20 minutes after the addition is complete. When the mixture is cooled, a precipitate of the expected product is obtained, and this is drained, made into a paste in water and then recrystallized from 96° strength alcohol. It melts at 172° C.

后处理

  1. additionhas been added
  2. temperatureHeating
  3. temperatureis maintained for 20 minutes
  4. additionafter the addition
  5. temperatureWhen the mixture is cooled

来源与证据

ORD记录
ord-0f00b2a48ac44f1f81b28c45b15724f2
来源数据集
uspto-grants-1988_02
专利号
US04727192

关联笔记

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