Ethyl Acetate → HCID 15949593、化合物

HRID 548715ノート

反応式

HRID 548715 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:14]=[C:15]([O:17][C@@H:18]([CH3:22])[CH2:19][O:20][CH3:21])[CH:16]=1)[C:5]([NH:7][C:8]1[CH:12]=[CH:11][N:10]([CH3:13])[N:9]=1)=[O:6].F[C:24]1[CH:37]=[CH:36][C:27]2[C:28](=[O:35])[N:29]([CH3:34])[C:30]([CH3:33])([CH3:32])[O:31][C:26]=2[CH:25]=1.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>C(#N)C>[CH3:22][C@H:18]([O:17][C:15]1[CH:14]=[C:4]([CH:3]=[C:2]([O:1][C:24]2[CH:37]=[CH:36][C:27]3[C:28](=[O:35])[N:29]([CH3:34])[C:30]([CH3:33])([CH3:32])[O:31][C:26]=3[CH:25]=2)[CH:16]=1)[C:5]([NH:7][C:8]1[CH:12]=[CH:11][N:10]([CH3:13])[N:9]=1)=[O:6])[CH2:19][O:20][CH3:21]

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 57663228HCID 57663228、化合物HCID 591271783-hydroxy-5-{[(2S)-1-methoxypropan-2-yl]oxy}-N-(1-methyl-1H-pyrazol-3-yl)benzamide

生成物 1

HCID 15949593HCID 15949593、化合物収率 30.1%

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 3-hydroxy-5-[(1S)-2-methoxy-(1-methylethyl)oxy]-N-(1-methyl-1H-pyrazol-3-yl)benzamide (0.25 g, 0.82 mmol), 7-fluoro-2,2,3-trimethyl-2,3-dihydro-4H-1,3-benzoxazin-4-one (172 mg, 0.82 mmol) and potassium carbonate (226 mg, 1.64 mmol) in acetonitrile (5 mL) was stirred in a microwave reactor at 160° C. for 12 hours. The mixture was reduced in vacuo and ethyl acetate (50 mL) added. The mixture was washed with water (50 mL), brine (50 mL), dried (MgSO4), and reduced in vacuo to give a brown oil which was chromatographed on silica, eluting with 0-10% methanol in DCM, to give the desired compound as a white foam (122 mg).

後処理

  1. additionadded
  2. washThe mixture was washed with water (50 mL), brine (50 mL)
  3. dry with materialdried (MgSO4)
  4. customto give a brown oil which
  5. customwas chromatographed on silica
  6. washeluting with 0-10% methanol in DCM

出典と根拠

ORDレコード
ord-e226c6586c7d490388e5675892cc3427
出典データセット
uspto-grants-2011_05
特許番号
US07943607B2

反応ノート

読み込み中…