Sodium Hydroxide → HCID 14624991、化合物

HRID 703447ノート

反応式

HRID 703447 の反応式
Cl[CH2:2][CH2:3][CH:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[NH:7][C:6](=[O:14])[CH2:5]1.[CH3:15][O:16][C:17]1[CH:26]=[C:25]2[C:20]([CH:21]=[CH:22][CH:23]=[C:24]2[N:27]2[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]2)=[CH:19][CH:18]=1.[OH-].[Na+]>ClCCl>[CH3:15][O:16][C:17]1[CH:26]=[C:25]2[C:20]([CH:21]=[CH:22][CH:23]=[C:24]2[N:27]2[CH2:28][CH2:29][N:30]([CH2:2][CH2:3][CH:4]3[C:13]4[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=4)[NH:7][C:6](=[O:14])[CH2:5]3)[CH2:31][CH2:32]2)=[CH:19][CH:18]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 145667201-(7-Methoxynaphthalen-1-yl)piperazineHCID 14624973HCID 14624973、化合物

生成物 1

HCID 14624991HCID 14624991、化合物収率 87.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
130 °C

実験手順

1.5 g (7.15 mmol) of (±)-4-(2-chloroethyl)-3,4-dihydro-2(1H)-quinolinone are mixed intimately with 3.65 g (15 mmol) of 1-(7-methoxy-1-naphthyl)piperazine and the mixture is heated to 130° C. for 1 h while stirring. The cooled residue is taken up between 25 ml of 2N sodium hydroxide and twice 50 ml of dichloromethane. The organic extract is washed with water, dried over magnesium sulphate and concentrated. The residue is purified by elution with a dichloromethane/methanol (95:5) mixture on a silica column. The purified fraction is crystallized in ether and this solid is drained and dried. 2.6 g (87.5%) of (±)-4-{2-[4-(7-methoxy-1-naphthyl)-1-piperazinyl]ethyl}-3,4-dihydro-2(1H)-quinolinone, melting point 177°-178° C., are obtained.

後処理

  1. extractionThe organic extract
  2. washis washed with water
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated
  5. customThe residue is purified by elution with a dichloromethane/methanol (95:5) mixture on a silica column
  6. customThe purified fraction is crystallized in ether
  7. customdried

出典と根拠

ORDレコード
ord-99a2bcedfc4a4c248e5482ec2af3d8e0
出典データセット
uspto-grants-1991_01
特許番号
US04983607

反応ノート

読み込み中…