6-Bromonaphthalene-2-sulfonyl chloride → 1-(6-Bromonaphthalene-2-sulfonyl)-4-(4-diisopropylaminomethylbenzoyl)piperazine

HRID 278593ノート

反応式

HRID 278593 の反応式
[CH:1]([N:4]([CH2:8][C:9]1[CH:22]=[CH:21][C:12]([C:13]([N:15]2[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]2)=[O:14])=[CH:11][CH:10]=1)[CH:5]([CH3:7])[CH3:6])([CH3:3])[CH3:2].[Br:23][C:24]1[CH:25]=[C:26]2[C:31](=[CH:32][CH:33]=1)[CH:30]=[C:29]([S:34](Cl)(=[O:36])=[O:35])[CH:28]=[CH:27]2>C(=O)([O-])O.[Na+].C(OCC)(=O)C>[Br:23][C:24]1[CH:25]=[C:26]2[C:31](=[CH:32][CH:33]=1)[CH:30]=[C:29]([S:34]([N:18]1[CH2:19][CH2:20][N:15]([C:13](=[O:14])[C:12]3[CH:21]=[CH:22][C:9]([CH2:8][N:4]([CH:5]([CH3:7])[CH3:6])[CH:1]([CH3:2])[CH3:3])=[CH:10][CH:11]=3)[CH2:16][CH2:17]1)(=[O:36])=[O:35])[CH:28]=[CH:27]2

参加物

5

反応物 2

HCID 144577416-Bromonaphthalene-2-sulfonyl chlorideHCID 226279521-(4-Diisopropylaminomethylbenzoyl)piperazine

生成物 1

HCID 226279921-(6-Bromonaphthalene-2-sulfonyl)-4-(4-diisopropylaminomethylbenzoyl)piperazine収率 59.9%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

To a mixture of 1-(4-diisopropylaminomethylbenzoyl)piperazine (200 mg) in 10% sodium hydrogen carbonate solution (10 ml) and ethyl acetate (15 ml), was added 6-bromonaphthalene-2-sulfonylchloride (179 mg), and the solution was stirred at room temperature for 30 minutes. The organic layer was separated, washed with water and extracted with 1 N hydrochloric acid. The extract was made alkaline with sodium hydroxide solution and extracted with dichloromethane. The extract was dried and concentrated. The residue was crystallized with ether to give the title compound (201 mg), as colorless crystals.

後処理

  1. customThe organic layer was separated
  2. washwashed with water
  3. extractionextracted with 1 N hydrochloric acid
  4. extractionextracted with dichloromethane
  5. customThe extract was dried
  6. concentrationconcentrated
  7. customThe residue was crystallized with ether

出典と根拠

ORDレコード
ord-7207ae2e68a44ed68f7c777a00adbed8
出典データセット
uspto-grants-2002_03
特許番号
US06359134B1

反応ノート

読み込み中…