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Sulfuric Acid → Ethyl (4S)-2-ethyl-8-(methoxy)-6-[methoxy(oxo)acetyl]-4-methyl-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazine-7-carboxylate

HRID 494117
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HRID 494117 반응식
Br[C:2]1[N:6]2[C@@H:7]([CH3:14])[CH2:8][N:9]([CH2:12][CH3:13])[C:10](=[O:11])[C:5]2=[C:4]([O:15][CH3:16])[C:3]=1[C:17]([O:19][CH2:20][CH3:21])=[O:18].[Li]CCCC.CCCCCC.[C:33](OC)(=[O:38])[C:34]([O:36][CH3:37])=[O:35].S(=O)(=O)(O)O>C1COCC1>[CH2:12]([N:9]1[CH2:8][C@H:7]([CH3:14])[N:6]2[C:2]([C:33](=[O:38])[C:34]([O:36][CH3:37])=[O:35])=[C:3]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:4]([O:15][CH3:16])=[C:5]2[C:10]1=[O:11])[CH3:13]
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참가 물질

7

반응물 5

HCID 1118Sulfuric AcidHCID 8058HexaneHCID 11120Dimethyl oxalateHCID 86624798(S)-Ethyl 6-bromo-2-ethyl-8-methoxy-4-methyl-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazine-7-carboxylateHCID 178418339Butyllithium

생성물 1

HCID 86612122
Ethyl (4S)-2-ethyl-8-(methoxy)-6-[methoxy(oxo)acetyl]-4-methyl-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazine-7-carboxylate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

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온도
-78 °C

실험 절차

To a cold (−78° C.) solution of ethyl (4S)-6-bromo-2-ethyl-8-methoxy-4-methyl-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazin-7-carboxylate (8.51 g, 23.7 mmol) in anhydrous THF (800 mL) under an atmosphere of dry nitrogen, a solution of n-BuLi in hexane (10.5 mL, 26.3 mmol, 2.5 M) was added. The resultant mixture was stirred at −78° C. for 20 minutes. A solution of dimethyl oxalate (6.4 g, 53.8 mmol; dried from concentration from benzene under vac) in anhydrous THF (30 mL) was added. The reaction mixture was stirred at −78° C. for 1 hour and cannulated into a mixture of aqueous sulfuric acid (240 mL, 2M) and THF (200 mL) maintained between at −5 to −35° C. The mixture was extracted with ethyl acetate (3 times). The organic extracts were combined, washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated under vacuum. The residue was subjected to column chromatography on silica gel eluted with 40 to 100% ethyl acetate-hexane gradient. Collection and concentration of appropriate fractions provided the titled compound.

후처리

  1. temperaturemaintained between at −5 to −35° C
  2. extractionThe mixture was extracted with ethyl acetate (3 times)
  3. washwashed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum
  7. washeluted with 40 to 100% ethyl acetate-hexane gradient
  8. customCollection and concentration of appropriate fractions

출처 및 근거

ORD 기록
ord-74c6e6b42a784af0a284bcb2b826298e
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07538112B2

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