Hydrochloric Acid → KR-33494

HRID 547513노트

반응식

HRID 547513 반응식
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

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59234712HCID 59234712, 화합물

생성물 1

HCID 25009726KR-33494수율 92.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-66f88ff83c7d4c028f7916c615ca13e0
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07939550B2

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