Hydrogen Bromide → 1-[7-Chloro-3-(3,5-dimethylphenyl)-2-oxo-4-(2-piperidin-2-yl-ethoxy)-1,2-dihydroquinolin-6-yl]-3-ethylurea

HRID 1857601노트

반응식

HRID 1857601 반응식
C(OC([N:11]1[CH2:16][CH2:15][CH2:14][CH2:13][CH:12]1[CH2:17][CH2:18][O:19][C:20]1[C:29]2[C:24](=[CH:25][C:26]([Cl:36])=[C:27]([NH:30][C:31]([NH:33][CH2:34][CH3:35])=[O:32])[CH:28]=2)[NH:23][C:22](=[O:37])[C:21]=1[C:38]1[CH:43]=[C:42]([CH3:44])[CH:41]=[C:40]([CH3:45])[CH:39]=1)=O)C1C=CC=CC=1.Br>C(O)(=O)C>[Cl:36][C:26]1[CH:25]=[C:24]2[C:29]([C:20]([O:19][CH2:18][CH2:17][CH:12]3[CH2:13][CH2:14][CH2:15][CH2:16][NH:11]3)=[C:21]([C:38]3[CH:39]=[C:40]([CH3:45])[CH:41]=[C:42]([CH3:44])[CH:43]=3)[C:22](=[O:37])[NH:23]2)=[CH:28][C:27]=1[NH:30][C:31]([NH:33][CH2:34][CH3:35])=[O:32]

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 538466182-{2-[7-Chloro-3-(3,5-dimethylphenyl)-6-(3-ethylureido)-2-oxo-1,2-dihydroquinolin-4-yloxy]-ethyl}-piperidine-1-carboxylic acid benzyl ester

생성물 1

HCID 98920381-[7-Chloro-3-(3,5-dimethylphenyl)-2-oxo-4-(2-piperidin-2-yl-ethoxy)-1,2-dihydroquinolin-6-yl]-3-ethylurea

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 2-{2-[7-chloro-3-(3,5-dimethylphenyl)-6-(3-ethylureido)-2-oxo-1,2-dihydroquinolin-4-yloxy]-ethyl}-piperidine-1-carboxylic acid benzyl ester (50 mg in 5 mL of a 30% solution of hydrobromic acid in acetic acid) was stirred at room temperature for 18 hours then concentrated in vacuo. The residue was treated with saturated sodium bicarbonate and then extracted with methylene chloride. Purification of the concentrate by flash chromatography on silica gel (methylene chloride:methanol:ammonium hydroxide, 96:3:1) gave the title compound (18 mg). MASS: 497 (M+H)

후처리

  1. concentrationthen concentrated in vacuo
  2. additionThe residue was treated with saturated sodium bicarbonate
  3. extractionextracted with methylene chloride
  4. customPurification of the
  5. concentrationconcentrate by flash chromatography on silica gel (methylene chloride:methanol:ammonium hydroxide, 96:3:1)

출처 및 근거

ORD 기록
ord-26eb1a2f6d554767be3ead844a136e19
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06147088

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