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ethyl oxo((phenylmethyl){[(3S)-4-(phenylmethyl)-3-morpholinyl]methyl}amino)acetate → (S)-8-Benzylhexahydropyrazino[2,1-C][1,4]oxazine-6,7-dione

HRID 419388
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HRID 419388 반응식
[O:1]=[C:2]([N:8]([CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[CH2:9][C@H:10]1[CH2:15][O:14][CH2:13][CH2:12][N:11]1CC1C=CC=CC=1)[C:3](OCC)=[O:4]>[Pd].CCOC(C)=O>[C:24]1([CH2:23][N:8]2[C:2](=[O:1])[C:3](=[O:4])[N:11]3[C@H:10]([CH2:15][O:14][CH2:13][CH2:12]3)[CH2:9]2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 66649783ethyl oxo((phenylmethyl){[(3S)-4-(phenylmethyl)-3-morpholinyl]methyl}amino)acetate

생성물 1

HCID 59452568(S)-8-Benzylhexahydropyrazino[2,1-C][1,4]oxazine-6,7-dione수율 54%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

1-Phenyl-N-{[(3S)-4-(phenylmethyl)-3-morpholinyl]methyl}methanamine (4.35 g, 14.7 mmol) and diisopropylethylamine (3.30 mL, 19.1 mmol) in THF (50 mL) cooled to 0° C. Ethylchlorooxo-acetate (1.80 mL, 16.2 mmol) was added dropwise via syringe. The ice bath was removed and the reaction was stirred at rt for 2 h. The reaction mixture was concentrated, taken up in EtOAc and washed with half saturated NaHCO3. The aqueous layer was back extracted with EtOAc, dried over MgSO4 and azeotroped in EtOH to provide ethyl oxo((phenylmethyl){[(3S)-4-(phenylmethyl)-3-morpholinyl]methyl}amino)acetate (5.83 g, 14.7 mmol, used without further purification). Ethyl oxo((phenylmethyl){[(3S)-4-(phenylmethyl)-3-morpholinyl]methyl}amino)acetate (5.83 g, 14.7 mmol) was hydrogenated (1 atm.) with Pd on carbon (1.18 g, 20% w/w with starting morpholine) for 13 days. The reaction was filtered through Celite® and washed thoroughly with MeOH. The solution was concentrated and subsequently triturated with EtOAc providing the title compound of step E (2.06 g, 7.9 mmol, 54% over two steps). 1H NMR (400 MHz, CDCl3) δ ppm 3.00 (ddd, J=13.9, 12.3, 4.2 Hz, 1H), 3.14-3.23 (m, 3H), 3.49 (td, J=12.1, 2.9 Hz, 1H), 3.72-3.82 (m, J=10.0, 10.0, 6.3, 4.0 Hz, 1H), 3.87 (dd, J=11.4, 3.7 Hz, 1H), 4.02 (dd, J=11.7, 4.4 Hz, 1H), 4.28 (dd, J=13.9, 2.2 Hz, 1H), 4.61-4.67 (m, 1H), 4.70-4.75 (m, 1H), 7.26-7.38 (m, 5H). Chiral HPLC analysis (Chiralpak AS-H, 4.6×150 mm, methanol (0.1% isopropyl amine), 1.0 mL/min, UV 254 nm, 25° C.) ee=99%, retention time, S=2.99 min. [α]D20° C.=−9.0:I=100 mm, c=0.975 in CHCl3.

후처리

  1. customfor 13 days
  2. filtrationThe reaction was filtered through Celite®
  3. washwashed thoroughly with MeOH
  4. concentrationThe solution was concentrated

출처 및 근거

ORD 기록
ord-adc03d396ed54cc5888e191d835b53e5
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08093239B2

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