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Formic Acid → (9AS)-Hexahydropyrazino-[2,1-c][1,4]oxazin-4(3H)-one

HRID 2063317
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HRID 2063317 반응식
[O:1]=[C:2]1[CH2:7][O:6][CH2:5][C@@H:4]2[CH2:8][N:9](C(OCC3C=CC=CC=3)=O)[CH2:10][CH2:11][N:3]12.C(O)=O.C([O-])=O.[NH4+]>C(O)C.[Pd]>[CH2:5]1[C@@H:4]2[CH2:8][NH:9][CH2:10][CH2:11][N:3]2[C:2](=[O:1])[CH2:7][O:6]1
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참가 물질

6

반응물 3

HCID 284Formic AcidHCID 2723923Ammonium formateHCID 16124472benzyl (9aS)-4-oxohexahydropyrazino[2,1-c][1,4]oxazine-8(1H)-carboxylate

생성물 1

HCID 16124477(9AS)-Hexahydropyrazino-[2,1-c][1,4]oxazin-4(3H)-one

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매
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온도
120 °C

실험 절차

Benzyl (9aS)-4-oxohexahydropyrazino[2,1-c][1,4]oxazine-8(1H)-carboxylate (0.19 g, 0.65 mmol was dissolved in ethanol (20 mL). The solution was transferred to a 25 mL vial, which contained 10% palladium on carbon (0.1 g), formic acid (0.1 g, 2.2 mmol) and ammonium formate (0.2 g, 3.17 mmol). The mixture was heated for 5 min at 120° C. using microwave single node heating. The catalyst was filtered off and the solution of crude (9aS)-hexahydropyrazino[2,1-c][1,4]oxazin-4(3H)-one was used in the next step without purification and quantification.

후처리

  1. temperatureheating
  2. filtrationThe catalyst was filtered off
  3. customthe solution of crude (9aS)-hexahydropyrazino[2,1-c][1,4]oxazin-4(3H)-one was used in the next step without purification and quantification

출처 및 근거

ORD 기록
ord-ea54da427c924e96b8e39e87b012a42a
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08288370B2

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