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 → HCID 19011942、化合物

HRID 1729301
ノート
印刷プレビュー

反応式

HRID 1729301 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.C([Li])CCC.CCCCCC.[C:33]([Cl:41])(=[O:40])[C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1>O1CCCC1>[ClH:41].[C:33]([C:21]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH2:15][CH2:14][N:11]1[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1)(=[O:40])[C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=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 4

HCID 7412Benzoyl chlorideHCID 8058HexaneHCID 21993766tert-Butyl 4-(2-phenylethyl)piperazine-1-carboxylateHCID 178418339Butyllithium

生成物 1

HCID 19011942HCID 19011942、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1.1 g of 1-(t-butyloxycarbonyl)-4-(2-phenylethyl)piperazine was dissolved in 8 ml of tetrahydrofuran, and 2.8 ml of butyllithium (1.6N, a hexane solution) was added dropwise to the solution at -30° C. followed by stirring for 30 minutes. Next, 0.88 ml of benzoyl chloride was added thereto, and the solution was stirred for 3 hours, poured into ice water, and then extracted with 50 ml of chloroform. The resultant chloroform layer was washed with water, dried over anhydrous sodium sulfate, and then concentrated, and the residue was separated through a silica gel column chromatograph (hexane/ethyl acetate=1/1). The resultant oil dissolved in 10 ml of ether, and 4.8 ml of a 4N hydrochloric acid/dioxane solution was added thereto, followed by stirring at room temperature for 30 minutes. The precipitated crystals were collected by filtration, whereby 0.36 g of 1-2-[2-benzoylphenyl]ethyl)piperazine.hydrochloride was obtained.

後処理

  1. stirringthe solution was stirred for 3 hours
  2. extractionextracted with 50 ml of chloroform
  3. washThe resultant chloroform layer was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customthe residue was separated through a silica gel column chromatograph (hexane/ethyl acetate=1/1)
  7. dissolutionThe resultant oil dissolved in 10 ml of ether
  8. addition4.8 ml of a 4N hydrochloric acid/dioxane solution was added
  9. stirringby stirring at room temperature for 30 minutes
  10. filtrationThe precipitated crystals were collected by filtration, whereby 0.36 g of 1-2-[2-benzoylphenyl]ethyl)piperazine.hydrochloride
  11. customwas obtained

出典と根拠

ORDレコード
ord-4bcadc8e0ad84a6ca1b431ac558c93c1
出典データセット
uspto-grants-1994_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05332739

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