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

HRID 13650

反応式

HRID 13650 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([I:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[C:12](OC(=O)C)(=O)[CH3:13]>>[I: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 72911Benzoic acid, 2-amino-5-iodo-

生成物 1

HCID 9153906-Iodo-2-methyl-4H-3,1-benzoxazin-4-one収率 90%

実験手順

2-Amino-5-iodobenzoic acid (25.4 g, 96.6 mmol) was added in portions to cold acetic anhydride (100 mL). The suspension was first stirred without cooling, then the resulting thick precipitate was heated at reflux for 1 h (red solution). 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 25.1 g (90%) of beige crystals. MS: m/z=287 (M).

後処理

  1. temperaturewithout cooling
  2. temperaturethe resulting thick precipitate was heated
  3. temperatureat reflux for 1 h (red solution)
  4. customThe product crystallized spontaneously
  5. temperatureupon cooling
  6. stirringAfter stirring in ice for 30 min
  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-f1525804138841f4a88333612dbe8237
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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