Hydrochloric Acid → KR-33494

HRID 547513ノート

反応式

HRID 547513 の反応式
C[O:2][C:3]([C:5]1[C:9]([NH:10][C:11](=[O:21])[CH2:12][S:13][C:14]2[CH:19]=[CH:18][C:17]([Br:20])=[CH:16][CH:15]=2)=[CH:8][N:7]([CH2:22][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[N:6]=1)=[O:4].[OH-].[Na+].Cl>CO>[Br:20][C:17]1[CH:18]=[CH:19][C:14]([S:13][CH2:12][C:11]([NH:10][C:9]2[C:5]([C:3]([OH:4])=[O:2])=[N:6][N:7]([CH2:22][CH2:23][C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH:8]=2)=[O:21])=[CH:15][CH:16]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59234712HCID 59234712、化合物

生成物 1

HCID 25009726KR-33494収率 92.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

100 mg (0.2 mM) of the compound obtained in Example 1 was dissolved in 1 ml of methanol to which 0.3 ml (0.3 mM, 1.5 eq) of 1N sodium hydroxide was added dropwise, and the resulting mixture was heated with stirring under a nitrogen atmosphere for 1 hour. The resultant was acidified with 1N hydrochloric acid solution, and extracted with ethyl acetate and brine. The organic solvent layer was dried over anhydrous sodium sulfate, filtered, and then distilled under reduced pressure, to obtain 90 mg (91.5%) of the title compound.

後処理

  1. additionwas added dropwise
  2. temperaturethe resulting mixture was heated
  3. extractionextracted with ethyl acetate and brine
  4. dry with materialThe organic solvent layer was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. distillationdistilled under reduced pressure

出典と根拠

ORDレコード
ord-66f88ff83c7d4c028f7916c615ca13e0
出典データセット
uspto-grants-2011_05
特許番号
US07939550B2

反応ノート

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