HRID1252024

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID313

Hydrochloric Acid

ClH

HCID14798

Sodium Hydroxide

HNaO

2 次

HCID82157

Nitrosylsulfuric acid

HNO5S

HCID5284359

未命名化合物

HCID14122483

N-(4-Chloro-3-hydroxyphenyl)acetamide

C8H8ClNO2

结构：CS(=O)(=O)c1cc(S(=O)(=O)[O-])ccc1N.CS(=O)(=O)c1cc(S(=O)(=O)[O-])ccc1N.[Ca+2]

HCID14122484

未命名化合物

PRODUCTS

生成物

结构：CC(=O)Nc1cc(O)c(Cl)cc1N=Nc1ccc(S(=O)(=O)[O-])cc1S(C)(=O)=O.CC(=O)Nc1cc(O)c(Cl)cc1N=Nc1ccc(S(=O)(=O)[O-])cc1S(C)(=O)=O.[Ca+2]

HCID136342787

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID6342

Acetonitrile

C2H3N

PROCEDURE

实验过程

A solution containing 18.6 g (0.1 mole) of 5-acetylamino-2-chlorophenol, 100 ml of 0.2 N sodium hydroxide, and 50 ml of acetonitrile was maintained at a temperature of 5° C. or less with stirring. Separately, 32.4 g (0.12 mole) of calcium 4-amino-3-methylsulfonylphenylsulfonate was diazotized with nitrosylsulfuric acid in the routine manner and the resulting diazo solution was added in portions to the above solution. After completion of the addition, 0.2N sodium hydroxide was added dropwise with ice-cooling unil the pH of the mixture became 4 to 5. After 30 minutes, the reaction mixture was adjusted to a pH value not exceeding 2 with 36% hydrochloric acid and 100 g of calcium chloride was added for salting-out. The crystalline precipitate was collected by filtration, washed with 50 ml of methanol and dried.

WORKUP

后处理

temperaturewas maintained at a temperature of 5° C. or less
additionwas added dropwise with ice-
temperaturecooling
additionwas added for salting-out
filtrationThe crystalline precipitate was collected by filtration
washwashed with 50 ml of methanol
customdried

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-98d5cca047ef4475bca1a29fa64ad33f
来源数据集: uspto-grants-1988_05
DOI: 10.6084/m9.figshare.5104873.v1
专利: US04741997
来源说明: uspto-grants-1988_05

反应 SMILES

[C:1]([NH:4][C:5]1[CH:6]=[CH:7][C:8]([Cl:12])=[C:9]([OH:11])[CH:10]=1)(=[O:3])[CH3:2].[OH-].[Na+].[NH2:15][C:16]1[CH:21]=[CH:20][C:19]([S:22]([O-:25])(=[O:24])=[O:23])=[CH:18][C:17]=1[S:26]([CH3:29])(=[O:28])=[O:27].[Ca+2:30].[NH2:31][C:32]1[CH:37]=[CH:36][C:35]([S:38]([O-:41])(=[O:40])=[O:39])=[CH:34][C:33]=1[S:42]([CH3:45])(=[O:44])=[O:43].[N:46](OS(=O)(=O)O)=O.Cl.[Cl-].[Ca+2].[Cl-]>C(#N)C>[CH3:29][S:26]([C:17]1[CH:18]=[C:19]([S:22]([O-:25])(=[O:23])=[O:24])[CH:20]=[CH:21][C:16]=1[N:15]=[N:31][C:6]1[CH:7]=[C:8]([Cl:12])[C:9]([OH:11])=[CH:10][C:5]=1[NH:4][C:1](=[O:3])[CH3:2])(=[O:28])=[O:27].[Ca+2:30].[CH3:45][S:42]([C:33]1[CH:34]=[C:35]([S:38]([O-:41])(=[O:39])=[O:40])[CH:36]=[CH:37][C:32]=1[N:31]=[N:46][C:6]1[CH:7]=[C:8]([Cl:12])[C:9]([OH:11])=[CH:10][C:5]=1[NH:4][C:1](=[O:3])[CH3:2])(=[O:44])=[O:43]