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Nitric Acid → N-(5-Chloro-2-hydroxy-3-nitrophenyl)acetamide

HRID 29858
ノート
印刷プレビュー

反応式

HRID 29858 の反応式
S(=O)(=O)(O)O.[Cl:6][C:7]1[CH:8]=[CH:9][C:10]([OH:17])=[C:11]([NH:13][C:14](=[O:16])[CH3:15])[CH:12]=1.[N+:18]([O-])([OH:20])=[O:19]>O>[Cl:6][C:7]1[CH:8]=[C:9]([N+:18]([O-:20])=[O:19])[C:10]([OH:17])=[C:11]([NH:13][C:14](=[O:16])[CH3:15])[CH:12]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 944Nitric Acid2 回HCID 1118Sulfuric Acid2 回HCID 952582-Acetylamino-4-chlorophenol

生成物 1

HCID 22142329N-(5-Chloro-2-hydroxy-3-nitrophenyl)acetamide

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
25 °C

実験手順

224.5 g of sulphuric acid (50% w/w) was dissolved in 300 ml of water and cooled to 25° C. while stirring under a mild nitrogen purge. 185.1 g (1 mole) of N-(5-chloro-2-hydroxyphenyl)acetamide prepared according to Example 1a was added to the diluted sulphuric acid and mixed intensively. 4 ml of nitric acid 65% w/w was added to the foam formed on top of the reaction mixture at low stirring speed. The stirring speed was increased and 75 ml of nitric acid 65% w/w was added in 45 minutes, while maintaining the temperature between 23 and 26° C. The mixture was stirred vigorously for an additional 1 hour at 23-26° C. Then the mixture was cooled to 0-5° C. and vigorously stirred at this temperature for 1 hour. The solid was filtered off quickly, washed three times with 300 ml of cold water, sucked for at least 30 minutes and dried at 50° C. and 100 mbar under a gentle nitrogen stream till dry.

後処理

  1. custompurge
  2. additionmixed intensively
  3. customformed on top of the reaction mixture at low stirring speed
  4. temperatureThe stirring speed was increased
  5. temperaturewhile maintaining the temperature between 23 and 26° C
  6. stirringThe mixture was stirred vigorously for an additional 1 hour at 23-26° C
  7. temperatureThen the mixture was cooled to 0-5° C.
  8. stirringvigorously stirred at this temperature for 1 hour
  9. filtrationThe solid was filtered off quickly
  10. washwashed three times with 300 ml of cold water
  11. waitsucked for at least 30 minutes
  12. customdried at 50° C.
  13. customtill dry

出典と根拠

ORDレコード
ord-ccd13ade850745d4aaf7dc82903a0142
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07423040B2

反応ノート

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