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Isobutyryl chloride → 8-Isobutyryloxy-6-oxo-5,6-dihydro-pyrido[2,3-b]pyrazine-7-carboxylic acid methyl ester

HRID 2197508
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반응식

HRID 2197508 반응식
[CH3:1][O:2][C:3]([C:5]1[C:14](=[O:15])[NH:13][C:8]2=[N:9][CH:10]=[CH:11][N:12]=[C:7]2[C:6]=1[OH:16])=[O:4].[C:17](Cl)(=[O:21])[CH:18]([CH3:20])[CH3:19]>ClCCCl>[CH3:1][O:2][C:3]([C:5]1[C:14](=[O:15])[NH:13][C:8]2=[N:9][CH:10]=[CH:11][N:12]=[C:7]2[C:6]=1[O:16][C:17](=[O:21])[CH:18]([CH3:20])[CH3:19])=[O:4]
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참가 물질

4

반응물 2

HCID 62325Isobutyryl chlorideHCID 57998840Methyl 8-hydroxy-6-oxo-5,6-dihydropyrido[2,3-b]pyrazine-7-carboxylate

생성물 1

HCID 581149228-Isobutyryloxy-6-oxo-5,6-dihydro-pyrido[2,3-b]pyrazine-7-carboxylic acid methyl ester

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

To a suspension of 8-hydroxy-6-oxo-5,6-dihydro-pyrido[2,3-b]pyrazine-7-carboxylic acid methyl ester (Example 7.1) in 1,2-dichloro-ethane (9 ml) was added powdered molecular sieves (4A) followed by dropwise addition of isobutyryl chloride (0.048 ml). The reaction mixture was heated to reflux for 5 hours, cooled to ambient temperature and filtered. The filtrate was concentrated to give 8-isobutyryloxy-6-oxo-5,6-dihydro-pyrido[2,3-b]pyrazine-7-carboxylic acid methyl ester as a light brown solid (0.166 g) which was used without further purification.

후처리

  1. additionwas added
  2. temperatureThe reaction mixture was heated
  3. temperatureto reflux for 5 hours
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-56b1a109e92940b3a48283ac9674653f
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08338598B2

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