Triethylamine → HCID 67390971, 화합물

HRID 1040459노트

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HRID 1040459 반응식
[C:1]([O:5][C:6]([NH:8][C@@H:9]([CH3:13])[C:10]([OH:12])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:14][O:15][C:16](=[O:25])[CH:17]([NH2:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(CC)CC>CN(C=O)C>[CH3:14][O:15][C:16](=[O:25])[CH:17]([NH:24][C:10](=[O:12])[C@@H:9]([NH:8][C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])[CH3:13])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 85082Tert-butoxycarbonylalanineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 10909919Methyl 2-amino-2-(pyridin-2-YL)acetate

생성물 1

HCID 67390971HCID 67390971, 화합물수율 98.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To (S)-2-tert-Butoxycarbonylamino-propionic acid (1.54 g, 8.12 mmol), Amino-pyridin-2-yl-acetic acid methyl ester (1.35 g, 8.12 mmol) and HATU (3.1 g, 8.12 mmol) was added the DMF (20 mL) and Et3N (2.26 ml, 16.20 mmol) and the solution was stirred for 2 h. The mixture was concentrated to remove most of the DMF was removed. The resulting oil was dissolved in EtOAc, washed with water, 0.1 N HCl aq., 1 N NaHCO3 aq., followed by Brine. The combined organics were dried over MgSO4, filtered, and concentrated in vacuo to provide ((S)-2-tert-Butoxycarbonylamino-propionylamino)-pyridin-2-yl-acetic acid methyl ester (2.7 g, 98%) as a yellow oil, m/z 338.61 [M+1]+

후처리

  1. concentrationThe mixture was concentrated
  2. customto remove most of the DMF
  3. customwas removed
  4. dissolutionThe resulting oil was dissolved in EtOAc
  5. washwashed with water, 0.1 N HCl aq., 1 N NaHCO3 aq.
  6. dry with materialThe combined organics were dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-ab885b42c7994a54af42b776cd43bf3d
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552205B2

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