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Dimethylformamide → 3-[[(2,3-Dihydro-1,4-benzodioxin-2-yl)methyl]ethylamino]propoxyl-2H-1-benzopyran-2-one

HRID 374228
ノート
印刷プレビュー

反応式

HRID 374228 の反応式
[CH2:1]([NH:3][CH2:4][CH:5]1[O:10][C:9]2[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=2[O:7][CH2:6]1)[CH3:2].BrCCCO[C:20]1[CH:29]=[C:28]2[C:23]([CH:24]=[CH:25][C:26](=[O:30])[O:27]2)=[CH:22][CH:21]=1.C(N([CH:37]([CH3:39])C)CC)(C)C.CN([CH:43]=[O:44])C>>[O:10]1[C:9]2[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=2[O:7][CH2:6][CH:5]1[CH2:4][N:3]([CH2:37][CH3:39])[CH2:1][CH2:2][CH2:43][O:44][C:25]1[C:26](=[O:30])[O:27][C:28]2[CH:29]=[CH:20][CH:21]=[CH:22][C:23]=2[CH:24]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 30614N-Ethyl-2,3-dihydro-1,4-benzodioxin-2-methanamineHCID 81531DiisopropylethylamineHCID 27571767-(3-bromopropoxy)-2H-chromen-2-one

生成物 1

HCID 867463753-[[(2,3-Dihydro-1,4-benzodioxin-2-yl)methyl]ethylamino]propoxyl-2H-1-benzopyran-2-one

反応条件

温度
76 °C

実験手順

N-Ethyl-2,3-dihydro-1,4-benzodioxin-2-methanamine (4.67 g, 24.2 mmole), 7-(3-bromopropoxy)coumarin (6.92 g, 24.4 mmole), and diisopropylethylamine (6.70 ml, 38.5 mmole) were combined in 300 ml of DMF and heated at 76° C. for 24 hours under a nitrogen atmosphere. The solvent was then removed in vacuum and replaced with dichloromethane. The mixture was washed with an equal volume of saturated aqueous sodium bicarbonate, dried over magnesium sulfate, filtered and concentrated in vacuum. The residue (10 g) was column chromatographed on 225 g of silica gel using 40% ethyl acetate/dichloromethane as eluant. The product-containing fractions were concentrated in vacuum and the residue crystallized from isopropanol with the addition of 30 ml of 4N isopropanolic HCl to give 4.94 g of the title compound as a white solid, monohydrochloride, m.p. 147°-152° C.

後処理

  1. customThe solvent was then removed in vacuum
  2. washThe mixture was washed with an equal volume of saturated aqueous sodium bicarbonate
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuum
  6. customchromatographed on 225 g of silica gel using 40% ethyl acetate/dichloromethane as eluant
  7. concentrationThe product-containing fractions were concentrated in vacuum
  8. customthe residue crystallized from isopropanol with the addition of 30 ml of 4N isopropanolic HCl

出典と根拠

ORDレコード
ord-9d3a2665dc6e43e8a41a8848147d1e03
出典データセット
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05166367

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート