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Hydrochloric Acid → HCID 23508042, 화합물

HRID 1883545
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HRID 1883545 반응식
CO.C([O:5][C:6]([C:8]1[C:9]([NH:16][C:17]2[CH:18]=[C:19]3[C:23](=[CH:24][CH:25]=2)[NH:22][N:21]=[CH:20]3)=[N:10][C:11]([S:14][CH3:15])=[N:12][CH:13]=1)=[O:7])C.[OH-].[Na+].Cl>O>[NH:22]1[C:23]2[C:19](=[CH:18][C:17]([NH:16][C:9]3[C:8]([C:6]([OH:7])=[O:5])=[CH:13][N:12]=[C:11]([S:14][CH3:15])[N:10]=3)=[CH:25][CH:24]=2)[CH:20]=[N:21]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 11209679HCID 11209679, 화합물

생성물 1

HCID 23508042HCID 23508042, 화합물수율 97.1%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To the solution of methanol (80 ml) was added the 4-(1H-5-indazolylamino)-2-methylthio-5-pyrimidinecarboxylic acid ethyl ester (5 g) obtained by the preparation example 1, and the solution was hydrolyzed at 40-50° C. for 1 hr, adding H2O (30 ml) and3N aq. NaOH (15 ml). The reaction mixture was cooled, measured pH 5 at 20° C., slowly adding 3 N aq. HCl. And then the reaction mixture was slowly added H2O (100 ml),stirred at 20° C. for 1 hr, filtered, washed with H2O (30 ml), and obtained a solid product. The solid product was dried at 50° C. in vacuo to obtain the desired compound (4.44 g, 97%).

후처리

  1. customobtained by the preparation example 1
  2. temperatureThe reaction mixture was cooled
  3. customat 20° C.
  4. waitat 20° C. for 1 hr
  5. filtrationfiltered
  6. washwashed with H2O (30 ml)
  7. customobtained a solid product
  8. customThe solid product was dried at 50° C. in vacuo

출처 및 근거

ORD 기록
ord-557b2caf255249b6a4679657e2671858
출처 데이터셋
uspto-grants-2004_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06762189B1

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