Hydrochloric Acid → HCID 178465663, 화합물

HRID 15925노트

반응식

HRID 15925 반응식
Cl.[C:2](=[NH:7])(OCC)[CH3:3].CCN(CC)CC.[Br:15][C:16]1[CH:21]=[CH:20][C:19]([NH:22][C:23]2[C:24]([C:32]([NH:34][NH2:35])=[O:33])=[CH:25][N:26]([CH3:31])[C:27](=[O:30])[C:28]=2[F:29])=[C:18]([F:36])[CH:17]=1.Cl>CN(C=O)C.C1COCC1>[NH:7]=[C:2]([NH:35][NH:34][C:32]([C:24]1[C:23]([NH:22][C:19]2[CH:20]=[CH:21][C:16]([Br:15])=[CH:17][C:18]=2[F:36])=[C:28]([F:29])[C:27](=[O:30])[N:26]([CH3:31])[CH:25]=1)=[O:33])[CH3:3]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 2724290Ethanimidic acid, ethyl ester, hydrochloride (1:1)HCID 666737984-(4-Bromo-2-fluorophenylamino)-5-fluoro-1-methyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid hydrazide

생성물 1

HCID 178465663HCID 178465663, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

실험 절차

Ethyl acetimidate HCl salt (40 mg, 0.32 mmol) and Et3N (0.049 mL, 0.35 mmol) were added to a stirred suspension of 4-(4-bromo-2-fluorophenylamino)-5-fluoro-1-methyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid hydrazide (0.10 g, 0.27 mmol) in 2:1 THF:DMF (3 mL) at 0° C. After 1.5 hours at 0° C. and 17 hours at room temperature, the reaction mixture was poured onto water, neutralized with dilute aqueous HCl and extracted with ethyl acetate. The combined organic extracts were dried (MgSO4) and concentrated under reduced pressure. Trituration with methylene chloride gave the desired product.

후처리

  1. customat 0° C
  2. addition17 hours at room temperature, the reaction mixture was poured onto water
  3. extractionextracted with ethyl acetate
  4. dry with materialThe combined organic extracts were dried (MgSO4)
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d064fa3d7f794633bb3fcbaf9288f1b6
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732616B2

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