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

HRID 12502노트

반응식

HRID 12502 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-67e561b31978414c8fcba4efacbbcbe9
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728018B2

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