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Ethyl Acetate → methyl 3-[(3-methyl-4-oxo-3,4-dihydro-2H-1,3-benzoxazin-7-yl)oxy]-5-[(3S)-tetrahydrofuran-3-yloxy]benzoate

HRID 548735
ノート
印刷プレビュー

反応式

HRID 548735 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([O:12][C@H:13]2[CH2:17][CH2:16][O:15][CH2:14]2)[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].F[C:19]1[CH:30]=[CH:29][C:22]2[C:23](=[O:28])[N:24]([CH3:27])[CH2:25][O:26][C:21]=2[CH:20]=1.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>C(#N)C>[CH3:27][N:24]1[C:23](=[O:28])[C:22]2[CH:29]=[CH:30][C:19]([O:1][C:2]3[CH:3]=[C:4]([CH:9]=[C:10]([O:12][C@H:13]4[CH2:17][CH2:16][O:15][CH2:14]4)[CH:11]=3)[C:5]([O:7][CH3:8])=[O:6])=[CH:20][C:21]=2[O:26][CH2:25]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

6

反応物 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 576631937-Fluoro-3-methyl-2,3-dihydro-4H-1,3-benzoxazin-4-oneHCID 59127189Methyl 3-hydroxy-5-{[(3S)-oxolan-3-yl]oxy}benzoate

生成物 1

HCID 57663180methyl 3-[(3-methyl-4-oxo-3,4-dihydro-2H-1,3-benzoxazin-7-yl)oxy]-5-[(3S)-tetrahydrofuran-3-yloxy]benzoate収率 39%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
160 °C

実験手順

A mixture of methyl 3-hydroxy-5-[(3S)-tetrahydrofuran-3-yloxy]benzoate (184 mg, 0.77 mmol), 7-fluoro-3-methyl-2,3-dihydro-4H-1,3-benzoxazin-4-one (140 mg, 0.77 mmol) and potassium carbonate (214 mg, 1.54 mmol) in acetonitrile (5 mL) was stirred in a microwave reactor at 160° C. for 10 hours then reduced in vacuo and ethyl acetate (50 mL) added. The organics were washed with brine (50 mL), dried (MgSO4), and reduced in vacuo and the crude oil purified by chromatography on silica, eluting with 30%-80% ethyl acetate in isohexane, to give the desired compound as a colourless oil (0.12 g).

後処理

  1. additionadded
  2. washThe organics were washed with brine (50 mL)
  3. dry with materialdried (MgSO4)
  4. customthe crude oil purified by chromatography on silica
  5. washeluting with 30%-80% ethyl acetate in isohexane

出典と根拠

ORDレコード
ord-d69d1368e58643e6a4cb1ea3eb09a20b
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07943607B2

反応ノート

読み込み中…

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