8-Methylenespiro[4.5]decane → 3-[(3-Methylphenyl)ethynyl]-1-oxa-2-azadispiro[4.2.4.2]tetradec-2-ene

HRID 2040890ノート

反応式

HRID 2040890 の反応式
[OH:1][N:2]=[C:3](Cl)[C:4]#[C:5][C:6]1[CH:7]=[C:8]([CH3:12])[CH:9]=[CH:10][CH:11]=1.[CH2:14]=[C:15]1[CH2:24][CH2:23][C:18]2([CH2:22][CH2:21][CH2:20][CH2:19]2)[CH2:17][CH2:16]1>>[CH3:12][C:8]1[CH:7]=[C:6]([C:5]#[C:4][C:3]2[CH2:14][C:15]3([CH2:16][CH2:17][C:18]4([CH2:19][CH2:20][CH2:21][CH2:22]4)[CH2:23][CH2:24]3)[O:1][N:2]=2)[CH:11]=[CH:10][CH:9]=1

参加物

3

反応物 2

HCID 574938568-Methylenespiro[4.5]decaneHCID 86662877N-hydroxy-3-(m-tolyl)prop-2-ynimidoyl chloride

生成物 1

HCID 566444373-[(3-Methylphenyl)ethynyl]-1-oxa-2-azadispiro[4.2.4.2]tetradec-2-ene

実験手順

The title compound was prepared following the procedure described for Compound 3c, using Compound 91d instead of Compound 3b and Compound 89a instead of Compound 3a. After the usual work-up procedure, the residue was purified by means of automated flash chromatography (ISOLERA®TM-Biotage; gradient Petroleum Ether-EtOAc from 97:3 to 9:1) to give the title compound as a white-yellowish solid. Yield: 55.8%.

後処理

  1. customThe title compound was prepared
  2. customAfter the usual work-up procedure, the residue was purified by means of automated flash chromatography (ISOLERA®TM-Biotage; gradient Petroleum Ether-EtOAc from 97:3 to 9:1)

出典と根拠

ORDレコード
ord-6163f8e566004cc097db5b08b8600e4e
出典データセット
uspto-grants-2013_11
特許番号
US08580962B2

反応ノート

読み込み中…