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

3-Methyl-2-butanone → HCID 71736007、化合物

HRID 579399
ノート
印刷プレビュー

反応式

HRID 579399 の反応式
[I:1][C:2]1[CH:3]=[C:4]([NH:9]N)[CH:5]=[C:6]([I:8])[CH:7]=1.[CH3:11][CH:12]([CH3:16])[C:13](=O)[CH3:14]>C(O)(=O)C>[I:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[C:4]2[C:3]=1[C:12]([CH3:16])([CH3:11])[C:13]([CH3:14])=[N:9]2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 112513-Methyl-2-butanoneHCID 86695330HCID 86695330、化合物

生成物 1

HCID 71736007HCID 71736007、化合物収率 61.9%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

2 g of 3,5-diiodophenylhydrazine (5.5 mmol), and 1 mL (9.3 mmol) of 3-methyl-2-butanone were refluxed in 15 mL of acetic acid for 20 hours. The acetic acid was evaporated and the residue was dissolved in ether. Insoluble precipitate was filtered off, and the etheric solution was washed with aqueous solutions of NaHCO3, followed by Na2S2O3 and water. The organic layer was dried with CaCl2 and ether was removed under reduced pressure by a rotary evaporator to give 1.4 g of 4,6-diiodo-2,3,3-trimethyl-3H-indole. 1H-NMR (200 MHz, DMSO-d6), δ, ppm: 7.92 (1H, d, 1.1 Hz, arom.), 7.79 (1H, d, 1.1 Hz, arom.), 2.22 (3H, s, 2-CH3), 1.32 (6H, s, C(CH3)2).

後処理

  1. customThe acetic acid was evaporated
  2. dissolutionthe residue was dissolved in ether
  3. filtrationInsoluble precipitate was filtered off
  4. washthe etheric solution was washed with aqueous solutions of NaHCO3
  5. dry with materialThe organic layer was dried with CaCl2 and ether
  6. customwas removed under reduced pressure by a rotary evaporator

出典と根拠

ORDレコード
ord-72f1a86e7be74f79a3a705a552980148
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09040721B2

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