Water → Ethyl 1-(2,4-dimethoxybenzyl)-7-(2-hydroxymethylpiperidin-1-yl)-4-oxo-1,4-dihydro-[1,8]naphthyridine-3-carboxylate

HRID 1867937ノート

反応式

HRID 1867937 の反応式
Cl[C:2]1[N:11]=[C:10]2[C:5]([C:6](=[O:28])[C:7]([C:23]([O:25][CH2:26][CH3:27])=[O:24])=[CH:8][N:9]2[CH2:12][C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:14]=2[O:21][CH3:22])=[CH:4][C:3]=1F.N1([CH2:36][OH:37])CCCCC1.[CH:38](N(C(C)C)CC)([CH3:40])[CH3:39].O.[C:48](#[N:50])[CH3:49]>>[CH3:22][O:21][C:14]1[CH:15]=[C:16]([O:19][CH3:20])[CH:17]=[CH:18][C:13]=1[CH2:12][N:9]1[C:10]2[C:5](=[CH:4][CH:3]=[C:2]([N:50]3[CH2:40][CH2:38][CH2:39][CH2:49][CH:48]3[CH2:36][OH:37])[N:11]=2)[C:6](=[O:28])[C:7]([C:23]([O:25][CH2:26][CH3:27])=[O:24])=[CH:8]1

参加物

6

反応物 5

HCID 962WaterHCID 6342AcetonitrileHCID 81531DiisopropylethylamineHCID 446909Piperidin-1-ylmethanolHCID 13937202Ethyl 7-chloro-1-(2,4-dimethoxybenzyl)-6-fluoro-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylate

生成物 1

HCID 69030307Ethyl 1-(2,4-dimethoxybenzyl)-7-(2-hydroxymethylpiperidin-1-yl)-4-oxo-1,4-dihydro-[1,8]naphthyridine-3-carboxylate

反応条件

温度
75 °C

実験手順

A mixture of EXAMPLE 1B (2.15 g), piperidinylmethanol (890 mg) and diisopropylethylamine (2.5 mL) in acetonitrile (50 mL) at 25° C. was stirred for 24 hours, heated at 75° C. for 5 days, cooled, treated with water, and extracted with dichloromethane (200 mL). The extract was washed with water and 1M hydrochloric acid and concentrated.

後処理

  1. temperaturecooled
  2. extractionextracted with dichloromethane (200 mL)
  3. washThe extract was washed with water and 1M hydrochloric acid
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-be7ac9be88d94205aa7e39f7e88acfe6
出典データセット
uspto-grants-2009_12
特許番号
US07632946B2

反応ノート

読み込み中…