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Pyridine → 2-ethoxy-6-(N-formyl-N-methylamino-methyl)-3,1-benzoxazin-4-one

HRID 557457
ノート
印刷プレビュー

反応式

HRID 557457 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([CH2:11][N:12]([CH:14]=[O:15])[CH3:13])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].N1C=CC=CC=1.Cl[C:23]([O:25][CH2:26][CH3:27])=O>O>[CH2:26]([O:25][C:23]1[O:5][C:4](=[O:6])[C:3]2[CH:7]=[C:8]([CH2:11][N:12]([CH:14]=[O:15])[CH3:13])[CH:9]=[CH:10][C:2]=2[N:1]=1)[CH3:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 10928Ethyl chloroformateHCID 580183122-amino-5-(N-formyl-N-methylamino-methyl)benzoic acid

生成物 1

HCID 580183142-ethoxy-6-(N-formyl-N-methylamino-methyl)-3,1-benzoxazin-4-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 6.0 g of 2-amino-5-(N-formyl-N-methylamino-methyl)-benzoic acid, there was added 30 mL of pyridine and then 11.1 mL of ethyl chloroformate was dropwise added to the mixture while ice-cooling the same. After the elapse of a night, 20 mL of water was dropwise added to the mixture to separate out a solid material, the solid was then isolated through filtration under reduced pressure and washed with 20 mL of water. Then the solid thus separated was dried under reduced pressure to give 3.97 g of the intended compound as a white solid.

後処理

  1. temperaturecooling the same
  2. customto separate out a solid material
  3. customthe solid was then isolated through filtration under reduced pressure
  4. washwashed with 20 mL of water
  5. customThen the solid thus separated
  6. customwas dried under reduced pressure

出典と根拠

ORDレコード
ord-4f2ba2d4773e4bb6860dd8adaa63da5d
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08058432B2

反応ノート

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