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

4-Bromo-1,2-dichlorobenzene → 1-(3,4-Dichloro-phenyl)-4-[4-(3-Piperidin-1-yl-propoxy)-phenyl]piperazine

HRID 1434584
ノート
印刷プレビュー

反応式

HRID 1434584 の反応式
[N:1]1([CH2:7][CH2:8][CH2:9][O:10][C:11]2[CH:16]=[CH:15][C:14]([N:17]3[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]3)=[CH:13][CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl:23][C:24]1[CH:25]=[C:26](Br)[CH:27]=[CH:28][C:29]=1[Cl:30].CC(C)([O-])C.[Na+].C1(P(C2C=CC=CC=2)C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1(C)C=CC=CC=1.C(OCC)(=O)C>[Cl:23][C:24]1[CH:25]=[C:26]([N:20]2[CH2:19][CH2:18][N:17]([C:14]3[CH:15]=[CH:16][C:11]([O:10][CH2:9][CH2:8][CH2:7][N:1]4[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]4)=[CH:12][CH:13]=3)[CH2:22][CH2:21]2)[CH:27]=[CH:28][C:29]=1[Cl:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 290134-Bromo-1,2-dichlorobenzeneHCID 634876Binap, (A+-)-HCID 99240131-[4-(3-Piperidin-1-ylpropoxy)phenyl]piperazineHCID 23676156Sodium t-butoxide

生成物 1

HCID 579357441-(3,4-Dichloro-phenyl)-4-[4-(3-Piperidin-1-yl-propoxy)-phenyl]piperazine

試薬・触媒・溶媒 2

HCID 1140
Toluene
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

Tris(dibenzylidineacetone) di palladium (0) (5 mol %; 23 mg) was added to a mixture of 1-[4-(3-piperidin-1-yl-propoxy)-phenyl]-piperazine (D11) (150 mg; 0.49 mmol), 3,4-dichloro bromo benzene (160 mg; 1.2 eq), sodium tert-butoxide (71 mg; 1.1 eq) and racemic 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (7.5 mol %; 24 mg) in dry toluene (3 ml). The resulting mixture was heated at reflux under argon for 18 hours. The reaction was allowed to cool to room temperature and diluted with ethyl acetate (10 ml). The resulting solids were removed by filtration and the filtrate evaporated in vacuo. The residue was purified by column chromatography on silica eluting with 3% methanol in dichloromethane to afford the title compound as a buff solid (45 mg)

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux under argon for 18 hours
  3. customThe resulting solids were removed by filtration
  4. customthe filtrate evaporated in vacuo
  5. customThe residue was purified by column chromatography on silica eluting with 3% methanol in dichloromethane

出典と根拠

ORDレコード
ord-d0f9f1e5b5ed42eabc20fea828ac68be
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07615550B2

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