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Hydrochloric Acid → HCID 12135422, 화합물

HRID 1270423
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HRID 1270423 반응식
C[O:2][C:3](=[O:19])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][CH2:11][C:12]1[CH:17]=[CH:16][C:15](=[O:18])[NH:14][CH:13]=1.[OH-].[Na+].Cl.C(O)C>CN(C)C=O>[O:18]=[C:15]1[NH:14][CH:13]=[C:12]([CH2:11][NH:10][C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([OH:19])=[O:2])[CH:17]=[CH:16]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric Acid2회HCID 702EthanolHCID 14798Sodium HydroxideHCID 693328462-[(6-Oxo-1,6-dihydro-pyridin-3-ylmethyl)-amino]-benzoic acid methyl ester

생성물 1

HCID 12135422HCID 12135422, 화합물수율 93.5%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

3.5 g (12.7 mmol) of 2-[(6-oxo-1,6-dihydro-pyridin-3-ylmethyl)-amino]-benzoic acid-methyl ester is mixed in 15 ml of dimethylformamide with 30 ml of 6N sodium hydroxide solution and stirred for 1.5 hours at room temperature. While being cooled with ice, it is then mixed with about 50 ml of 4N hydrochloric acid, the precipitation is suctioned off, and it is washed with water. 3.1 g, which is taken up in 29.3 ml of 1N sodium hydroxide solution and 142 ml of ethanol, is obtained, and it is heated for 1.5 hours to a bath temperature of 120° C. The ethanol is then drawn off in a vacuum, it is made acidic with 2N hydrochloric acid, and the precipitated product is suctioned off and dried well. 2.9 g (93.5% of theory) of 2-[(6-oxo-1,6-dihydro-pyridin-3-ylmethyl)-amino]-benzoic acid is obtained.

후처리

  1. temperatureWhile being cooled with ice, it
  2. customthe precipitation
  3. washit is washed with water
  4. custom142 ml of ethanol, is obtained
  5. temperatureit is heated for 1.5 hours to a bath temperature of 120° C
  6. customdried well

출처 및 근거

ORD 기록
ord-f9aa669250444c43959db2da3d1a7156
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07202260B2

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