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

Dimethylformamide → N-[3-(7-methoxyindol-3-yl)-2-propyl]-3-chloromandelamide

HRID 399018
ノート
印刷プレビュー

反応式

HRID 399018 の反応式
CN(C=O)C.[NH2:6][CH:7]([CH3:20])[CH2:8][C:9]1[C:17]2[C:12](=[C:13]([O:18][CH3:19])[CH:14]=[CH:15][CH:16]=2)[NH:11][CH:10]=1.[Cl:21][C:22]1[CH:23]=[C:24]([CH:30]=[CH:31][CH:32]=1)[CH:25]([OH:29])[C:26](O)=[O:27].F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1>C(OCC)(=O)C.C(N(CC)CC)C>[CH3:19][O:18][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]2[C:12]=1[NH:11][CH:10]=[C:9]2[CH2:8][CH:7]([NH:6][C:26](=[O:27])[CH:25]([C:24]1[CH:30]=[CH:31][CH:32]=[C:22]([Cl:21])[CH:23]=1)[OH:29])[CH3:20]
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 6228DimethylformamideHCID 859813-Chloromandelic acidHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 114242613-(2-Aminopropyl)-7-methoxyindole

生成物 1

HCID 18969567N-[3-(7-methoxyindol-3-yl)-2-propyl]-3-chloromandelamide収率 94.1%

試薬・触媒・溶媒 2

HCID 8471
Triethylamine
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a DMF solution (80 ml) containing 3-(2-aminopropyl)-7-methoxyindole (12.24 g) and 3-chloromandelic acid (7.46 g) is added benzotriazole-N-oxytris(dimethylamino)phosphonium hexafluorophosphate (17.68 g), and then thereto is added dropwise triethylamine (9.8 ml). The mixture is stirred at room temperature for five hours, and to the reaction mixture is added ethyl acetate. The mixture is washed successively with water, 10% aqueous citric acid solution, water, a saturated aqueous sodium hydrogen carbonate solution, water and a saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The mixture is evaporated to remove the solvent under reduced pressure, and the residue is purified by silica gel column chromatography (eluent; ethyl acetate/n-hexane=1:1→2:1) to give N-[3-(7-methoxyindol-3-yl)-2-propyl]-3-chloromandelamide (14.02 g) as an oily product.

後処理

  1. washThe mixture is washed successively with water, 10% aqueous citric acid solution, water
  2. dry with materiala saturated aqueous sodium hydrogen carbonate solution, water and a saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate
  3. customThe mixture is evaporated
  4. customto remove the solvent under reduced pressure
  5. customthe residue is purified by silica gel column chromatography (eluent; ethyl acetate/n-hexane=1:1→2:1)

出典と根拠

ORDレコード
ord-dd99aebcf126462dba15c564736a5726
出典データセット
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05817689

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