Acetic Anhydride → 1-Acetamido-7-naphthol

HRID 260667

反応式

HRID 260667 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[CH:10]=[C:9]([OH:12])[CH:8]=[CH:7]2.[C:13](OC(=O)C)(=[O:15])[CH3:14]>>[OH:12][C:9]1[CH:10]=[C:11]2[C:6]([CH:5]=[CH:4][CH:3]=[C:2]2[NH:1][C:13](=[O:15])[CH3:14])=[CH:7][CH:8]=1

参加物

3

反応物 2

HCID 7918Acetic AnhydrideHCID 83588-Amino-2-naphthalenol

生成物 1

HCID 809461-Acetamido-7-naphthol収率 98.3%

実験手順

100 g (0.55 mol) of 8-aminonaphth-2-ol are poured into 125 ml (135.25 g or 1.325 mol) of acetic anhydride cooled in an ice bath, and the mixture is stirred under cold conditions for 1 h. The mixture obtained is poured into 375 ml of ice-water and stirred for several hours. The violet solid is collected by filtration, washed three times with 30 ml of diethyl ether and dried under reduced pressure. 108.8 g of a product melting point: 193°-195° C. are obtained which is used as it is in the following step.

後処理

  1. temperaturecooled in an ice bath
  2. customThe mixture obtained
  3. stirringstirred for several hours
  4. filtrationThe violet solid is collected by filtration
  5. washwashed three times with 30 ml of diethyl ether
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-13936575bfc34ea29975b969b0f98d9f
出典データセット
uspto-grants-1996_06
特許番号
US05530002

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