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丁醇 → 3,4-Dibutoxy-3-cyclobutene

HRID 217221
笔记
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反应方程式

HRID 217221 反应方程式
[CH2:1]([OH:5])[CH2:2][CH2:3][CH3:4]>N1C=CC=CC=1>[CH2:1]([O:5][C:4]1[CH2:3][CH2:2][C:1]=1[O:5][CH2:1][CH2:2][CH2:3][CH3:4])[CH2:2][CH2:3][CH3:4]
参与物实验过程来源与证据反应笔记

参与物

3

反应物 1

HCID 263丁醇

产物 1

HCID 571803643,4-Dibutoxy-3-cyclobutene收率 12.2%

试剂、催化剂与溶剂 1

HCID 1049吡啶溶剂

实验过程

In a reactor flask purged with nitrogen gas, 1.4 g (2.0 mmol) of the compound No. 40 obtained in Example 2, 0.50 g (2.2 mmol) of 3,4-dibutoxy-3-cyclobutene, 4.0 g of butanol, and 0.24 g of pyridine were charged, and the resulting mixture was stirred at room temperature for 15 hours, at 50° C. for 4 hours, and at 75° C. for 21 hours. The reaction solution was cooled to room temperature and concentrated to dryness under reduced pressure. The resulting residue was purified with a column (silica gel, chloroform:acetone=10:1) to obtain 0.92 g of a brown amorphous product (yield: 70%). The brown amorphous product was subjected to the 1H-NMR analysis. The brown amorphous product was identified as the aimed product of compound No. 50. The result of the 1H-NMR analysis is shown below.

来源与证据

ORD记录
ord-aba85c85a6af4d90a2703b9db6c11882
本页导航参与物实验过程来源与证据反应笔记
来源数据集
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08193366B2

反应笔记

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