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

HRID 12502ノート

反応式

HRID 12502 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-67e561b31978414c8fcba4efacbbcbe9
出典データセット
uspto-grants-2010_06
特許番号
US07728018B2

反応ノート

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