Hydrochloric Acid → HCID 178465663、化合物

HRID 15925ノート

反応式

HRID 15925 の反応式
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]

参加物

7

反応物 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

生成物 1

HCID 178465663HCID 178465663、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d064fa3d7f794633bb3fcbaf9288f1b6
出典データセット
uspto-grants-2010_06
特許番号
US07732616B2

反応ノート

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