Ammonium Hydroxide → HCID 59234713, 화합물

HRID 547515노트

반응식

HRID 547515 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:9][C:10]([NH:12][C:13]2[C:14]([C:26](O)=[O:27])=[N:15][N:16]([CH2:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH:17]=2)=[O:11])=[CH:4][CH:3]=1.[NH4+:29].[OH-]>O1CCCC1.C(Cl)(=O)C(Cl)=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([S:8][CH2:9][C:10]([NH:12][C:13]2[C:14]([C:26]([NH2:29])=[O:27])=[N:15][N:16]([CH2:18][CH2:19][C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=3)[CH:17]=2)=[O:11])=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 14923Ammonium HydroxideHCID 25009726KR-33494

생성물 1

HCID 59234713HCID 59234713, 화합물수율 19%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 65578Oxalyl chloride용매

실험 절차

113 mg (0.3 mM) of the compound obtained in Example 23 was dissolved in 1 ml of tetrahydrofuran to which 60 μl (0.7 mM) of oxalyl chloride was added dropwise, and the resulting mixture was stirred under a nitrogen atmosphere for 30 minutes. Subsequently, 70 μl of NH4OH was added thereto, and the resulting mixture was stirred under a nitrogen atmosphere for 1 hour. The solvent was distilled off under reduced pressure, and the resultant was extracted with ethyl acetate and brine. The organic solvent layer was dried over anhydrous sodium sulfate, filtered, and then distilled under reduced pressure. The resulting impure compound was purified by column chromatography (hexane:ethyl acetate=2:1), to obtain 21 mg (19%) of the title compound.

후처리

  1. additionwas added dropwise
  2. stirringthe resulting mixture was stirred under a nitrogen atmosphere for 1 hour
  3. distillationThe solvent was distilled off under reduced pressure
  4. extractionthe resultant was extracted with ethyl acetate and brine
  5. dry with materialThe organic solvent layer was dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. distillationdistilled under reduced pressure
  8. customThe resulting impure compound was purified by column chromatography (hexane:ethyl acetate=2:1)

출처 및 근거

ORD 기록
ord-41f7026ebe40465ba8d1fe9a21c03d8c
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07939550B2

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