Cyclopentylhydrazine hydrochloride → HCID 10545058, 화합물

HRID 612404

반응식

HRID 612404 반응식
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

참가 물질

5

반응물 3

HCID 212349Cyclopentylhydrazine hydrochlorideHCID 10541431HCID 10541431, 화합물HCID 10942334Sodium Methoxide

생성물 1

HCID 10545058HCID 10545058, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6d77ae71d4524779bbe1745cc5b103ac
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06004974

연결된 노트

불러오는 중…