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Potassium Hydroxide → HCID 25190386, 화합물

HRID 219765
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HRID 219765 반응식
[F:1][C:2]([F:35])([F:34])[C:3]1[CH:11]=[C:10]([C:12]#[N:13])[CH:9]=[C:8]2[C:4]=1[C:5]([NH:22][C:23](=[O:33])[CH2:24][N:25]1[CH2:30][CH2:29][N:28]([CH2:31][CH3:32])[CH2:27][CH2:26]1)([C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=1)[C:6](=[O:14])[NH:7]2.[OH-:36].[K+]>CC(O)(C)C>[Cl:21][C:18]1[CH:17]=[CH:16][C:15]([C:5]2([NH:22][C:23](=[O:33])[CH2:24][N:25]3[CH2:26][CH2:27][N:28]([CH2:31][CH3:32])[CH2:29][CH2:30]3)[C:4]3[C:8](=[CH:9][C:10]([C:12]([NH2:13])=[O:36])=[CH:11][C:3]=3[C:2]([F:1])([F:34])[F:35])[NH:7][C:6]2=[O:14])=[CH:20][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 66602253HCID 66602253, 화합물

생성물 1

HCID 25190386HCID 25190386, 화합물수율 60.4%

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

0.16 g of the product obtained in Example 4, 0.47 g of potassium hydroxide and 7 ml of t-BuOH are placed in a round-bottomed flask equipped with a magnetic stirrer. The mixture is left to react at 50° C. for 5 hours. The resulting mixture is filtered through Celite and washed with THF. The filtrate is evaporated under vacuum and the residue is taken up in ethyl acetate and washed with water. The organic phase is dried over Na2SO4, filtered and evaporated under vacuum. 100 mg of an oil are obtained, which oil is purified by flash chromatography, eluting with 8/2 ethyl acetate/methanol. 10 mg of white solid are isolated.

후처리

  1. customequipped with a magnetic stirrer
  2. waitThe mixture is left
  3. customto react at 50° C. for 5 hours
  4. filtrationThe resulting mixture is filtered through Celite
  5. washwashed with THF
  6. customThe filtrate is evaporated under vacuum
  7. washwashed with water
  8. dry with materialThe organic phase is dried over Na2SO4
  9. filtrationfiltered
  10. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-a5f34ff25a584c5ba21faf4efbd1e5d1
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08202871B2

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