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Aluminium lithium hydride → HCID 67197085, 화합물

HRID 547516
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HRID 547516 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.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[Br:20][C:17]1[CH:18]=[CH:19][C:14]([S:13][CH2:12][C:11]([NH:10][CH:9]2[CH2:8][N:7]([CH2:22][CH2:23][C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)[N:6]=[C:5]2[CH2:3][OH:2])=[O:21])=[CH:15][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 59234712HCID 59234712, 화합물

생성물 1

HCID 67197085HCID 67197085, 화합물수율 68.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

150 mg (0.3 mM) of the compound obtained in Example 1 was dissolved in 2 ml of tetrahydrofuran to which 62 mg (0.9 mM) of lithium aluminum hydride was added dropwise at 0, and the resulting mixture was stirred at room temperature under a nitrogen atmosphere for 1 hour. After the reaction was terminated, the resultant was acidified with 1N hydrochloric acid solution, 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 96 mg (68.1%) of the title compound.

후처리

  1. additionwas added dropwise at 0
  2. customAfter the reaction was terminated
  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-6a12f9e0c4944b7e9c390257e5147654
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07939550B2

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