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 1857601ノート

反応式

HRID 1857601 の反応式
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]

参加物

4

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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)

後処理

  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)

出典と根拠

ORDレコード
ord-26eb1a2f6d554767be3ead844a136e19
出典データセット
uspto-grants-2000_11
特許番号
US06147088

反応ノート

読み込み中…