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

HRID 557457
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인쇄 미리보기

반응식

HRID 557457 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4f2ba2d4773e4bb6860dd8adaa63da5d
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08058432B2

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