4-Hydroxybenzaldehyde → HCID 86760174, 화합물

HRID 1792748노트

반응식

HRID 1792748 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.[Cl:10][C:11]1[N:16]=[N:15][C:14]([N:17]2[CH2:22][CH2:21][CH:20](CCO)[CH2:19][CH2:18]2)=[CH:13][CH:12]=1.[CH2:26](O)[CH3:27]>O>[Cl:10][C:11]1[N:16]=[N:15][C:14]([N:17]2[CH2:18][CH2:19][CH2:20][CH2:21][CH:22]2[CH2:26][CH2:27][O:1][C:2]2[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=2)=[CH:13][CH:12]=1

참가 물질

5

반응물 3

HCID 1264-HydroxybenzaldehydeHCID 702EthanolHCID 149892211-(6-Chloro-3-pyridazinyl)-4-piperidineethanol

생성물 1

HCID 86760174HCID 86760174, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

4- {2-[1-(6-Chloro-3-pyridazinyl)piperidinyl]ethoxy}benzaldehyde (Intermediate IIa) was prepared from 4-hydroxybenzaldehyde and 2-[1-(6-Chloro-3-pyridazinyl)-4-piperidinyl]ethanol using a Mitsunobu Reaction and following the general methods described in U.S. Pat. No. 4,992,433. The aldehyde (60 mg, 0.17 mmol) was dissolved in ethanol (5 ml) with stirring at room temperature and a solution of ethoxyanine in water (0.5 ml, 50% EtONH2) was added. The reaction was stirred at room temperature for 2 days and then concentrated on a rotary evaporator and the residue was purified by chromatography (silica gel 18g) using chloroform as eluent. The first compound to elute was the O-ethyloxime (1) which was obtained as a pale cream solid (30mg, 44%).

후처리

  1. customa Mitsunobu Reaction
  2. stirringThe reaction was stirred at room temperature for 2 days
  3. concentrationconcentrated on a rotary evaporator
  4. customthe residue was purified by chromatography (silica gel 18g)
  5. washThe first compound to elute

출처 및 근거

ORD 기록
ord-787609c5fc094e55af8b9d71496b9fb7
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07078403B1

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