Acetic Anhydride → 6-Bromo-2-methyl-4H-3,1-benzoxazin-4-one

HRID 13649

反応式

HRID 13649 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([Br:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[C:12](OC(=O)C)(=O)[CH3:13]>>[Br:11][C:8]1[CH:9]=[CH:10][C:2]2[N:1]=[C:12]([CH3:13])[O:5][C:4](=[O:6])[C:3]=2[CH:7]=1

参加物

3

反応物 2

HCID 7918Acetic AnhydrideHCID 798582-Amino-5-bromobenzoic acid

生成物 1

HCID 27971426-Bromo-2-methyl-4H-3,1-benzoxazin-4-one収率 85%

実験手順

2-Amino-5-bromobenzoic acid (25 g, 116 mmol) was added in portions to acetic anhydride (150 mL) giving a slightly exothermic reaction to 30° C. The suspension was heated at reflux for 2 h. The product crystallized spontaneously upon cooling. After stirring in ice for 30 min, the crystals were filtered off and washed twice with heptane. The crystals were thoroughly dried at 0.1 mbar/50° C. One obtained 22.4 g (85%) of beige crystals. MS: m/z=239/241 (M).

後処理

  1. customgiving
  2. customa slightly exothermic reaction to 30° C
  3. temperatureThe suspension was heated
  4. temperatureat reflux for 2 h
  5. customThe product crystallized spontaneously
  6. temperatureupon cooling
  7. filtrationthe crystals were filtered off
  8. washwashed twice with heptane
  9. customThe crystals were thoroughly dried at 0.1 mbar/50° C

出典と根拠

ORDレコード
ord-c8e59a2becb04486bdd9575972ab5d27
出典データセット
uspto-grants-2010_06
特許番号
US07728142B2

関連ノート

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