Hydrazine, acetate (1:1) → HCID 68863971, 화합물

HRID 494124노트

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HRID 494124 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]2[C:8]([C:18](=O)[C:19]([O:21][CH3:22])=[O:20])=[C:9]([C:13](OCC)=[O:14])[C:10]([O:11][CH3:12])=[C:4]2[C:3]1=[O:24].C(OC(NCC(N(CC(OC)OC)C)=O)=O)C1C=CC=CC=1.C(O)(=O)C.[NH2:51][NH2:52]>C(O)(=O)C>[CH3:12][O:11][C:10]1[C:9]2[C:13](=[O:14])[NH:52][N:51]=[C:18]([C:19]([O:21][CH3:22])=[O:20])[C:8]=2[N:5]2[CH2:6][CH2:7][N:2]([CH3:1])[C:3](=[O:24])[C:4]=12

참가 물질

5

반응물 3

HCID 165591Hydrazine, acetate (1:1)HCID 58009747HCID 58009747, 화합물HCID 68865401HCID 68865401, 화합물

생성물 1

HCID 68863971HCID 68863971, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
160 °C

실험 절차

A solution of ethyl 2-methyl-8-(methoxy)-6-[methoxy(oxo)acetyl]-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazine-7-carboxylate (1.28 g, 3.78 mmol; prepared in a manner similar to that described in Example 62, step 5 to 8, starting with 1-methylpiperazin-2-one (Example 7, step 1 to 3) and hydrazine acetate (1.05 g, 11.36 mmol) in glacial acetic acid (8 mL) was heated at 160° C. in an microwave oven for 20 minutes. The mixture was concentrated under vacuum. The residue was partitioned between chloroform and brine. The organic extract was dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum. The residue was triturated in a 4:1 mixture of ethanol and diethyl ether. The precipitate was filtered to afford the title compound. ES MS M+1=321

후처리

  1. customprepared in a manner similar to
  2. concentrationThe mixture was concentrated under vacuum
  3. customThe residue was partitioned between chloroform and brine
  4. extractionThe organic extract
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum
  8. customThe residue was triturated in a 4:1 mixture of ethanol and diethyl ether
  9. filtrationThe precipitate was filtered

출처 및 근거

ORD 기록
ord-91fb736e81e641519cdf14ef56ffe676
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538112B2

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