Hydrochloric Acid → HCID 178451126、化合物

HRID 84206

反応式

HRID 84206 の反応式
C([O:3][C:4](=O)[C@@:5]([OH:33])([CH3:32])[CH2:6][N:7]([CH2:17][C:18]1[CH:23]=[CH:22][C:21]([C:24]2[CH:29]=[C:28]([Cl:30])[CH:27]=[CH:26][C:25]=2[F:31])=[CH:20][CH:19]=1)[NH:8][C:9]([C:11]1[O:15][N:14]=[C:13]([OH:16])[CH:12]=1)=[O:10])C.[CH2:35]([OH:39])[CH:36]([CH3:38])[CH3:37].Cl.O1CCOCC1>>[CH2:35]([O:39][C:4](=[O:3])[C@@:5]([OH:33])([CH3:32])[CH2:6][N:7]([CH2:17][C:18]1[CH:19]=[CH:20][C:21]([C:24]2[CH:29]=[C:28]([Cl:30])[CH:27]=[CH:26][C:25]=2[F:31])=[CH:22][CH:23]=1)[NH:8][C:9]([C:11]1[O:15][N:14]=[C:13]([OH:16])[CH:12]=1)=[O:10])[CH:36]([CH3:38])[CH3:37]

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 6560IsobutanolHCID 312751,4-DioxaneHCID 178472219HCID 178472219、化合物

生成物 1

HCID 178451126HCID 178451126、化合物収率 100%

実験手順

(R)-3-[N-(5′-Chloro-2′-fluorobiphenyl-4-ylmethyl)-N′-(3-hydroxy-isoxazole-5-carbonyl)-hydrazino]-2-hydroxy-2-methyl-propionic acid ethyl ester (100 mg, 0.2 mmol) was dissolved in isobutyl alcohol (6 mL, 60 mmol), followed by the addition of 4 M HCl in dioxane (1 mL, 4 mmol). The resulting mixture was stirred at room temperature for 8 hours, then evaporated under reduced pressure and purified by preparative HPLC. The clean fractions were combined and lyophilized to yield the title compound (52 mg, 100% purity). MS m/z [M+H]+ calc'd for C25H27ClFN3O6, 520.16; Found 520.2.

後処理

  1. customevaporated under reduced pressure
  2. custompurified by preparative HPLC

出典と根拠

ORDレコード
ord-68e22f34ef574f2a8c6af34044b32293
出典データセット
uspto-grants-2014_09
特許番号
US08846913B2

関連ノート

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