Bromine → 7-bromo-2-methyl-2H-benzo[b][1,4]oxazin-3(4H)-one

HRID 840368ノート

反応式

HRID 840368 の反応式
[CH3:1][CH:2]1[C:7](=[O:8])[NH:6][C:5]2[CH:9]=[CH:10][CH:11]=[CH:12][C:4]=2[O:3]1.[Br:13]Br>C(O)(=O)C>[Br:13][C:11]1[CH:10]=[CH:9][C:5]2[NH:6][C:7](=[O:8])[CH:2]([CH3:1])[O:3][C:4]=2[CH:12]=1

参加物

4

反応物 2

HCID 24408BromineHCID 3017302-methyl-2H-1,4-benzoxazin-3(4H)-one

生成物 1

HCID 226231297-bromo-2-methyl-2H-benzo[b][1,4]oxazin-3(4H)-one

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

In 56 ml of glacial acetic acid, 6 g of 2-methyl-1,4-benzoxazin-3-(4H)-one is precooled at 0° C. and mixed drop by drop with 1.9 ml of bromine in 19 ml of glacial acetic acid. It is allowed to reach room temperature and stirred for another 8 hours. The mixture is poured onto ice water, the crystals are suctioned off and washed with water. 9.3 g of crude product results, which is recrystallized from ethanol/water. 7-Bromo-2-methyl-1,4-benzoxazin-3-(4H)-one is obtained as a by-product. As an alternative, 4-bromo-2-aminophenol can also be reacted according to the described processes.

後処理

  1. customis precooled at 0° C.
  2. customto reach room temperature
  3. additionThe mixture is poured onto ice water
  4. washwashed with water
  5. custom9.3 g of crude product results
  6. customwhich is recrystallized from ethanol/water

出典と根拠

ORDレコード
ord-69d59c62c7974ca8ade48f550e266db3
出典データセット
uspto-grants-2002_04
特許番号
US06365736B1

反応ノート

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