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Hydrochloric Acid → HCID 72794471、化合物

HRID 661722
ノート
印刷プレビュー

反応式

HRID 661722 の反応式
Cl.C(OC(=O)[NH:8][CH2:9][CH2:10][O:11][N:12]=[CH:13][C:14]1[CH:19]=[C:18]([C:20](=[O:26])[NH:21][O:22][CH2:23][CH2:24][OH:25])[C:17]([NH:27][C:28]2[CH:33]=[CH:32][C:31]([I:34])=[CH:30][C:29]=2[F:35])=[C:16]([F:36])[C:15]=1[F:37])(C)(C)C.C(=O)(O)[O-].[Na+]>C(OCC)(=O)C>[NH2:8][CH2:9][CH2:10][O:11][N:12]=[CH:13][C:14]1[C:15]([F:37])=[C:16]([F:36])[C:17]([NH:27][C:28]2[CH:33]=[CH:32][C:31]([I:34])=[CH:30][C:29]=2[F:35])=[C:18]([CH:19]=1)[C:20]([NH:21][O:22][CH2:23][CH2:24][OH:25])=[O:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 72964235{2-[2,3-Difluoro-4-(2-fluoro-4-iodo-phenylamino)-5-(2-hydroxy-ethoxycarbamoyl)-benzylideneaminooxy]-ethyl}-carbamic acid tert-butyl ester

生成物 1

HCID 72794471HCID 72794471、化合物収率 37%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

1 N HCl solution in ethyl acetate (1 ml) was added to a solution of {2-[2,3-difluoro-4-(2-fluoro-4-iodo-phenylamino)-5-(2-hydroxy-ethoxycarbamoyl)-benzylideneaminooxy]-ethyl}-carbamic acid tert-butyl ester (55 mg, 0.31 mmol) prepared in Process A in ethyl acetate (5 ml). This mixture was then stirred at room temperature for 1.5 hours. After the completion of the reaction, the reaction solution was neutralized with saturated sodium bicarbonate solution (50 ml) and extracted with ethyl acetate (100 ml×3). The extract was washed with saturated brine, and the organic layer was dried over anhydrous sodium sulfate and filtered. The solvent was evaporated off under reduced pressure, and the resulting residue was washed with diethyl ether (10 ml) and then recrystallized from methanol to give 5-[(2-amino-ethoxyimino)-methyl]-3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-benzamide (17.31 mg, 37% yield) as a pale yellow solid.

後処理

  1. customAfter the completion of the reaction
  2. extractionextracted with ethyl acetate (100 ml×3)
  3. washThe extract was washed with saturated brine
  4. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customThe solvent was evaporated off under reduced pressure
  7. washthe resulting residue was washed with diethyl ether (10 ml)
  8. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-380ced045d1647d697fd0b0e97ee4523
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084645B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート