Methanol → N-(2-amino-5-chloro-3-methylbenzoyl)-N'-methoxycarbonylhydrazine

HRID 251925ノート

反応式

HRID 251925 の反応式
[Cl:1][C:2]1[CH:13]=[C:12]([CH3:14])[C:5]2[NH:6]C(=O)O[C:9](=[O:10])[C:4]=2[CH:3]=1.[C:15]([O:19][CH3:20])(=[O:18])[NH:16][NH2:17].CO>O>[NH2:6][C:5]1[C:12]([CH3:14])=[CH:13][C:2]([Cl:1])=[CH:3][C:4]=1[C:9]([NH:17][NH:16][C:15]([O:19][CH3:20])=[O:18])=[O:10]

参加物

5

反応物 3

HCID 887MethanolHCID 80519Methyl carbazateHCID 115502595-Chloro-3-methyl isatoic anhydride

生成物 1

HCID 66854326N-(2-amino-5-chloro-3-methylbenzoyl)-N'-methoxycarbonylhydrazine収率 60.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 1.05 g of 6-chloro-8-methyl-1H-benzo[d]-1,3-oxazine-2,4-dione, 0.46 g of methyl carbazate and 20 ml of methanol was heated to reflux for 3 hours. After the reaction mixture was allowed to cool to around room temperature, water was poured thereto and the mixture was extracted with ethyl acetate three times. The resulting organic layer was concentrated under reduced pressure, and the residue was washed with toluene to obtain 0.77 g of N-(2-amino-5-chloro-3-methylbenzoyl)-N′-methoxycarbonylhydrazine of the formula:

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 3 hours
  3. temperatureto cool to around room temperature
  4. extractionthe mixture was extracted with ethyl acetate three times
  5. concentrationThe resulting organic layer was concentrated under reduced pressure
  6. washthe residue was washed with toluene

出典と根拠

ORDレコード
ord-edb1e9fb023140cda37768f2d9730a17
出典データセット
uspto-grants-2011_01
特許番号
US07867949B2

反応ノート

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