Sodium Hydroxide → HCID 14624991, 화합물

HRID 703447노트

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HRID 703447 반응식
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

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 145667201-(7-Methoxynaphthalen-1-yl)piperazineHCID 14624973HCID 14624973, 화합물

생성물 1

HCID 14624991HCID 14624991, 화합물수율 87.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
130 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-99a2bcedfc4a4c248e5482ec2af3d8e0
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04983607

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