Hydrochloric Acid → Phenyl N-(2-chloro-4-hydroxyphenyl)carbamate

HRID 557484ノート

反応式

HRID 557484 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][C:3]=1[Cl:9].N1C=CC=CC=1.Cl[C:17]([O:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[O:18].Cl>CN(C)C=O.C(OCC)(=O)C.O>[Cl:9][C:3]1[CH:4]=[C:5]([OH:8])[CH:6]=[CH:7][C:2]=1[NH:1][C:17](=[O:18])[O:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 15891Phenyl chloroformateHCID 871844-Amino-3-chlorophenol

生成物 1

HCID 11277058Phenyl N-(2-chloro-4-hydroxyphenyl)carbamate

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

After suspending 4-amino-3-chlorophenol (23.7 g) in N,N-dimethylformamide (100 mL) and adding pyridine (23.4 mL) while cooling on ice, phenyl chloroformate (23.2 ml) was added dropwise below 20° C. Stirring was performed at room temperature for 30 minutes, and then water (400 mL), ethyl acetate (300 mL) and 6N HCl (48 mL) were added, the mixture was stirred and the organic layer was separated. The organic layer was washed twice with 10% brine (200 mL), and dried over magnesium sulfate. The solvent was removed to give 46 g of the title compound as a solid.

後処理

  1. additionwas added dropwise below 20° C
  2. stirringthe mixture was stirred
  3. customthe organic layer was separated
  4. washThe organic layer was washed twice with 10% brine (200 mL)
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was removed

出典と根拠

ORDレコード
ord-8247a5cb9f064eb78fb9e3e7f27ebb65
出典データセット
uspto-grants-2011_11
特許番号
US08058474B2

反応ノート

読み込み中…