4-Methylmorpholine → Boc-Leu-Glu-OtBu

HRID 1943982

반응식

HRID 1943982 반응식
[NH:1]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[C@H:2]([C:7]([O:9]N1C(=O)CCC1=O)=O)[CH2:3][CH:4]([CH3:6])[CH3:5].[NH2:24][C@H:25]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:26][CH2:27][C:28](=[O:30])[OH:29].CN1CCOCC1>CN(C=O)C.CN(C1C=CN=CC=1)C>[NH:1]([C:17]([O:19][C:20]([CH3:21])([CH3:22])[CH3:23])=[O:18])[C@H:2]([C:7]([NH:24][C@H:25]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:26][CH2:27][C:28](=[O:29])[OH:30])=[O:9])[CH2:3][CH:4]([CH3:5])[CH3:6]

참가 물질

6

반응물 3

HCID 79724-MethylmorpholineHCID 1175051-(1,1-Dimethylethyl) hydrogen L-glutamateHCID 11023929Boc-Leu-OSu

생성물 1

HCID 87984260Boc-Leu-Glu-OtBu

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6228Dimethylformamide용매

실험 절차

To a solution of Boc-Leu-OSu and Glu-OtBu in DMF was added NMM and DMAP. The solution was stirred at ambient temperatures for 18 hours then the solvent was removed. Crude product was taken up in 100 ml CHCl3, washed 3× with pH 3 water (100 ml), once with water (100 ml) and once with brine (100 ml). Organic layer was dried with MgSO4 and filtered. Solvent was removed and solid was dried over vacuum. Solid was collected as a white powder (8.78 g, quant. yield, ˜80% purity TLC). Product was used directly without further characterization.

후처리

  1. customthe solvent was removed
  2. washwashed 3× with pH 3 water (100 ml)
  3. dry with materialOrganic layer was dried with MgSO4
  4. filtrationfiltered
  5. customSolvent was removed
  6. customsolid was dried over vacuum
  7. customSolid was collected as a white powder (8.78 g, quant. yield, ˜80% purity TLC)

출처 및 근거

ORD 기록
ord-0cf9c167a0c94a43be175ee458d26593
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08394813B2

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