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

Diisopropylamine → 2-(1-methyl-1H-indol-3-yl)pentanoic acid

HRID 590997
ノート
印刷プレビュー

反応式

HRID 590997 の反応式
[CH2:1]([Li])[CH2:2][CH2:3]C.C(NC(C)C)(C)C.[CH3:13][N:14]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:16]([CH2:23][C:24]([OH:26])=[O:25])=[CH:15]1.C(I)CC>O1CCCC1>[CH3:13][N:14]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:16]([CH:23]([CH2:1][CH2:2][CH3:3])[C:24]([OH:26])=[O:25])=[CH:15]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 7912DiisopropylamineHCID 336431-IodopropaneHCID 2541662-(1-methyl-1H-indol-3-yl)acetic acidHCID 178418339Butyllithium

生成物 1

HCID 708180292-(1-methyl-1H-indol-3-yl)pentanoic acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Under a nitrogen atmosphere, butyl lithium (1.6M, 10 mL, 16 mmol) was added at −78° C. to a solution of diisopropylamine (2.22 mL, 15.84 mmol) in anhydrous tetrahydrofurane. After 25 minutes, a solution of 1-methyl-3-indoleacetic acid (1 g, 5.28 mmol) in tetrahydrofurane (20 mL) was slowly added at −78° C., followed by the addition of propyliodide (1 mL, 10 mmol) after 45 minutes. The mixture was then warmed to room temperature and stirred for 2 hours. The mixture was quenched with water (2 mL) and concentrated in vacuo. The residue was diluted with water (20 mL) and washed with diethyl ether (20 mL). The organic layer was acidified with hydrochloric acid aqueous solution 1N to pH 3 and extracted with dichloromethane (3×10 mL). The organic layer was washed with brine, dried over sodium sulfate, filtered and evaporated under reduced pressure to afford the desired acid (12a) as a brown solid without further purification (1.22 g, 5.28 mmol, 100%).

後処理

  1. customThe mixture was quenched with water (2 mL)
  2. concentrationconcentrated in vacuo
  3. additionThe residue was diluted with water (20 mL)
  4. washwashed with diethyl ether (20 mL)
  5. extractionextracted with dichloromethane (3×10 mL)
  6. washThe organic layer was washed with brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-620df8915c9a4db1aae3863cc959264d
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09238026B2

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