Ethyl chloroformate → HCID 13365015、化合物

HRID 1249390ノート

反応式

HRID 1249390 の反応式
[CH2:1]([O:3][C:4](Cl)=[O:5])[CH3:2].[CH2:7]1[O:22][CH:10]([C:11]2[C:16]([O:17][CH3:18])=[C:15]([O:19][CH3:20])[CH:14]=[CH:13][C:12]=2[NH2:21])[O:9][CH2:8]1.[OH-].[Na+]>O1CCCC1.O>[CH2:8]1[O:9][CH:10]([C:11]2[C:16]([O:17][CH3:18])=[C:15]([O:19][CH3:20])[CH:14]=[CH:13][C:12]=2[NH:21][C:4]([O:3][CH2:1][CH3:2])=[O:5])[O:22][CH2:7]1

参加物

6

反応物 3

HCID 10928Ethyl chloroformateHCID 14798Sodium HydroxideHCID 133650142-(1,3-Dioxolan-2-yl)-3,4-dimethoxyaniline

生成物 1

HCID 13365015HCID 13365015、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Ethylchloroformate (1.9 g, 17.5 mM) is added with stirring to 2-amino-5,6-dimethoxybenzaldehyde-ethyleneketal (1.6 g, 7.1 mM) dissolved in tetrahydrofuran (50 ml). A solution of sodium hydroxide in H2O (0.72 g in 3.5 ml H2O) is added and the resulting solution is stirred for 2 hours at room temperature. The tetrahydrofuran is removed in vacuo and the residue extracted with CHCl3 (2×100 ml). The extracts are dried over Na2SO4, filtered, and the solvent removed in vacuo. The crude product is recrystallized from n-hexane; yield 1.2 g (57.1%); m.p. 95°-96° C.

後処理

  1. customThe tetrahydrofuran is removed in vacuo
  2. extractionthe residue extracted with CHCl3 (2×100 ml)
  3. dry with materialThe extracts are dried over Na2SO4
  4. filtrationfiltered
  5. customthe solvent removed in vacuo
  6. customThe crude product is recrystallized from n-hexane

出典と根拠

ORDレコード
ord-ddedcca97ff5468f83570dcf24172a7d
出典データセット
uspto-grants-1986_12
特許番号
US04631283

反応ノート

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