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Methylamine → 4-Methylaminomethyl-7-methoxycoumarin

HRID 1167050
ノート
印刷プレビュー

反応式

HRID 1167050 の反応式
[CH3:1][NH2:2].Br[CH2:4][C:5]1[C:14]2[C:9](=[CH:10][C:11]([O:15][CH3:16])=[CH:12][CH:13]=2)[O:8][C:7](=[O:17])[CH:6]=1.C(=O)([O-])[O-].[K+].[K+].ClCCl>O1CCCC1>[CH3:16][O:15][C:11]1[CH:10]=[C:9]2[C:14]([C:5]([CH2:4][NH:2][CH3:1])=[CH:6][C:7](=[O:17])[O:8]2)=[CH:13][CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6329MethylamineHCID 6344DichloromethaneHCID 11430Potassium Carbonate2 回HCID 1218944-Bromomethyl-7-methoxycoumarin

生成物 1

HCID 89318374-Methylaminomethyl-7-methoxycoumarin

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of methylamine in tetrahydrofuran (2M, 1.10 ml) was added to an ice-cooled mixture of 4-bromomethyl-7-methoxycoumarin (0.30 g), potassium carbonate (0.5 g) and dichloromethane (10 ml). The mixture was stirred at room temperature for 2 days then added to an aqueous solution of potassium carbonate. The organic phase was washed with water, dried (MgSO4) and evaporated. The residue was purified by chromatography on silica gel (eluent 10% methanol in dichloromethane), then crystallised from methanol to give the title compound as a white solid (0.14 g).

後処理

  1. temperaturecooled
  2. washThe organic phase was washed with water
  3. dry with materialdried (MgSO4)
  4. customevaporated
  5. customThe residue was purified by chromatography on silica gel (eluent 10% methanol in dichloromethane)
  6. customcrystallised from methanol

出典と根拠

ORDレコード
ord-65df06f0f0ab4220954f09c98c2ae949
出典データセット
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06617124B1

反応ノート

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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