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Diisopropylethylamine → HCID 67497107, 화합물

HRID 1628246
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HRID 1628246 반응식
Cl[C:2]1[CH:7]=[C:6]([C:8]2[CH:12]=[C:11]([NH:13][C:14](=[O:32])[C@@H:15]([NH:23][CH2:24][C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[N:10]([CH3:33])[N:9]=2)[CH:5]=[CH:4][N:3]=1.C(N(C(C)C)CC)(C)C>[Pd].CO>[CH3:33][N:10]1[C:11]([NH:13][C:14](=[O:32])[C@@H:15]([NH:23][CH2:24][C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:16][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)=[CH:12][C:8]([C:6]2[CH:5]=[CH:4][N:3]=[CH:2][CH:7]=2)=[N:9]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 81531DiisopropylethylamineHCID 86762560HCID 86762560, 화합물

생성물 1

HCID 67497107HCID 67497107, 화합물수율 61.7%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a 100 ml flask was added 1.4 g of 17.8.A, 500 mg of Pd on carbon, 150 ml of MeOH and 520 μl of diisopropylethylamine. The air was removed from the flask and replaced with hydrogen gas. This process was repeated four more times and then the reaction was stirred at room temperature for 2 hours, at which time the reaction was filtered over a bed of celite. The solvent was then removed and the crude was purified with a silica gel column (eluting with 2-5% MeOH in DCM) to give 800 mg of (S)-tert-butyl 2-(1-(1-methyl-3-(pyridin-4-yl)-1H-pyrazol-5-ylamino)-1-oxo-3-phenylpropan-2-ylamino)acetate 17.8.B as a solid. (Rf silica=0.27 in 5% MeOH in DCM).

후처리

  1. customThe air was removed from the flask
  2. filtrationwas filtered over a bed of celite
  3. customThe solvent was then removed
  4. customthe crude was purified with a silica gel column (eluting with 2-5% MeOH in DCM)

출처 및 근거

ORD 기록
ord-399b9f86e72840ad942975fbdeba62e4
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08785468B2

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