ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Benzoyl chloride → 1-(3,3-Dimethylpiperazin-1-yl)-4-phenylphthalazine

HRID 1689946
ノート
印刷プレビュー

反応式

HRID 1689946 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([N:12]2[CH2:17][CH2:16][NH:15][C:14]([CH3:19])([CH3:18])[CH2:13]2)=[N:4][N:3]=1.C(N(CC)CC)C.C(Cl)(=O)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>ClCCl.C(OCC)(=O)C>[CH3:18][C:14]1([CH3:19])[NH:15][CH2:16][CH2:17][N:12]([C:5]2[C:6]3[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=3)[C:2]([C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)=[N:3][N:4]=2)[CH2:13]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 7412Benzoyl chlorideHCID 8471TriethylamineHCID 575814821-Chloro-4-(3,3-dimethylpiperazin-1-yl)phthalazine

生成物 1

HCID 669047751-(3,3-Dimethylpiperazin-1-yl)-4-phenylphthalazine

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 1-chloro-4-(3,3-dimethylpiperazin-1-yl)phthalazine (540 mg, 2 mmol) in 10 mL of dichloromethane was added triethylamine (0.56 mL, 4 mmol, 2 eq), followed by benzoyl chloride (0.26 mL, 2.2 mmol, 1.1 eq). The reaction was stirred at rt for 30 min and diluted with 100 mL of ethyl acetate. The organic layer was washed with 1×10 mL of sat. NaHCO3 solution and 1×10 mL of sat. NaCl solution. Purification by column chromatography (100:2 dichloromethane:methanol) afforded 1-(3,3-dimethylpiperazin-1-yl)-4-phenylphthalazine (BSL-7). 1H-NMR (400 Mhz) δ 1.65 (s, 6H), 3.46 (s, 2H), 3.63 (m, 4H), 7.34 (m, 3H), 7.42 (m, 3H), 7.42 (m, 3H), 7.83 (m, 2H), 8.03 (m, 1H), 8.17 (m, 1H).

後処理

  1. washThe organic layer was washed with 1×10 mL of sat. NaHCO3 solution and 1×10 mL of sat. NaCl solution
  2. customPurification by column chromatography (100:2 dichloromethane:methanol)

出典と根拠

ORDレコード
ord-1c2e37f7cb244581bd4fb60cbaad75b4
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08153633B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート