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

1,4'-Bipiperidine → 4,5,6,7-Tetramethoxy-2-[3-[4-[(4-piperidinopiperidino)carbonyl]phenoxy]propyl]indan hydrochloride

HRID 2268488
ノート
印刷プレビュー

反応式

HRID 2268488 の反応式
[CH3:1][O:2][C:3]1[C:11]([O:12][CH3:13])=[C:10]([O:14][CH3:15])[C:9]([O:16][CH3:17])=[C:8]2[C:4]=1[CH2:5][CH:6]([CH2:18][CH2:19][CH2:20][O:21][C:22]1[CH:30]=[CH:29][C:25]([C:26]([OH:28])=O)=[CH:24][CH:23]=1)[CH2:7]2.[N:31]1([CH:37]2[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]2)[CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]1.[ClH:43].C(N=C=NCCCN(C)C)C.O.ON1C2C=CC=CC=2N=N1>C1COCC1.O.C(N(CC)CC)C>[ClH:43].[CH3:17][O:16][C:9]1[C:10]([O:14][CH3:15])=[C:11]([O:12][CH3:13])[C:3]([O:2][CH3:1])=[C:4]2[C:8]=1[CH2:7][CH:6]([CH2:18][CH2:19][CH2:20][O:21][C:22]1[CH:30]=[CH:29][C:25]([C:26]([N:40]3[CH2:41][CH2:42][CH:37]([N:31]4[CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]4)[CH2:38][CH2:39]3)=[O:28])=[CH:24][CH:23]=1)[CH2:5]2
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 786071,4'-BipiperidineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 183485514-[3-(4,5,6,7-Tetramethoxyindan-2-yl)propoxy]benzoic acid

生成物 1

HCID 183485344,5,6,7-Tetramethoxy-2-[3-[4-[(4-piperidinopiperidino)carbonyl]phenoxy]propyl]indan hydrochloride収率 98.4%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒

実験手順

The mixture of 4-[3-(4,5,6,7-tetramethoxyindan-2-yl)propoxy]benzoic acid (2.00 g), 4-piperidinopiperidine (1.62 g), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (1.84 g), 1-hydroxybenzotriazole monohydrate (1.47 g), and triethylamine (2.01 ml) in THF (40 ml) was stirred at room temperature for 12 hr. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride and dried. The solvent was removed in vacuo. The residue was purified by alumina column chromatography (hexane to hexane:ethyl acetate=1:2) and converted into its hydrochloride, which was further recrystallized from ethanol-diisopropylether to yield the entitled compound (2.85 g) as crystals.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water and saturated aqueous sodium chloride
  3. customdried
  4. customThe solvent was removed in vacuo
  5. customThe residue was purified by alumina column chromatography (hexane to hexane:ethyl acetate=1:2)
  6. customwas further recrystallized from ethanol-diisopropylether

出典と根拠

ORDレコード
ord-c62c12c3c1c245c7af11574d0b567a5d
出典データセット
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06326369B1

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