Cyclopentylhydrazine hydrochloride → HCID 10545058、化合物

HRID 612404

反応式

HRID 612404 の反応式
CO[C:3]1[C:4](=[O:21])[N:5]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15](OC)[CH:14]=2)[CH2:6][CH2:7][C:8]=1[C:9](=O)[CH2:10][CH3:11].Cl.[CH:23]1([NH:28][NH2:29])[CH2:27][CH2:26][CH2:25][CH2:24]1.[CH3:30][O-:31].[Na+]>C(O)C>[CH:23]1([N:28]2[C:3]3[C:4](=[O:21])[N:5]([C:13]4[CH:14]=[CH:15][C:16]([O:31][CH3:30])=[CH:17][CH:18]=4)[CH2:6][CH2:7][C:8]=3[C:9]([CH2:10][CH3:11])=[N:29]2)[CH2:27][CH2:26][CH2:25][CH2:24]1

参加物

5

反応物 3

HCID 212349Cyclopentylhydrazine hydrochlorideHCID 10541431HCID 10541431、化合物HCID 10942334Sodium Methoxide

生成物 1

HCID 10545058HCID 10545058、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A stirred mixture of 3-methoxy-1-(3-methoxyphenyl)-2-oxo-4-propionyl-1,2,5,6-tetrahydro-pyridine (0.49 grams, 1.7 mmole), cyclopentylhydrazine hydrochloride (0.40 grams) and sodium methoxide (46 mg, 0.85 mmole) in anhydrous ethanol was heated to reflux. After 16 hours, the mixture was concentrated under reduced pressure and chromatographed on a silica gel column using 1:4 ethyl acetate/hexane as eluent to give a white solid. Recrystallization from ether gave white needles. M.P. 64.65° C.; MS m/z [M+] 340.2025; HRMS [M+] 340.2046.

後処理

  1. temperaturewas heated to reflux
  2. concentrationthe mixture was concentrated under reduced pressure
  3. customchromatographed on a silica gel column
  4. customto give a white solid
  5. customRecrystallization from ether
  6. customgave white needles

出典と根拠

ORDレコード
ord-6d77ae71d4524779bbe1745cc5b103ac
出典データセット
uspto-grants-1999_12
特許番号
US06004974

関連ノート

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