Hydrazine hydrate (1:1) → 5-Methyl-3a,4,5,6,7,7a-hexahydro-1H-pyrazolo[4,3-c]pyridine

HRID 1024363노트

반응식

HRID 1024363 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]=[C:4]([CH:8]=O)[CH2:3]1.O.[NH2:11][NH2:12]>CCCCO>[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]2[NH:11][N:12]=[CH:8][CH:4]2[CH2:3]1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 154280611-Methyl-3,4-dehydropiperidine-3-carboxaldehyde

생성물 1

HCID 593393775-Methyl-3a,4,5,6,7,7a-hexahydro-1H-pyrazolo[4,3-c]pyridine

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

3.2 g 1-Methyl-1,2,5,6-tetrahydro-pyridine-3-carbaldehyde was dissolved in 10 mL n-BuOH. Added were 2 equiv. of hydrazine hydrate, the mixture was refluxed for 24 hours and subsequently concentrated in vacuo. The residue was taken up in DCM and extracted with 2M NaOH, and the organic phase was dried over Na2SO4, filtrated and concentrated in vacuo to yield 1.78 g of a brown oil which was used without further purification in the subsequent step.

후처리

  1. additionAdded
  2. temperaturethe mixture was refluxed for 24 hours
  3. concentrationsubsequently concentrated in vacuo
  4. extractionextracted with 2M NaOH
  5. dry with materialthe organic phase was dried over Na2SO4
  6. filtrationfiltrated
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-cbe888ed19cf41d8a1222e410537bb9e
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722887B2

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