Methanol → 8-(6-Acetyl-4-ethoxy-7-methyl-5,8-dihydropyrido[2,3-d]pyrimidin-5-yl)-2-methyl-4H-chromen-4-one

HRID 1947250ノート

反応式

HRID 1947250 の反応式
[C:1]([C:4]1[CH:5]([C:16]2[CH:17]=[CH:18][CH:19]=[C:20]3[C:25]=2[O:24][C:23]([CH3:26])=[CH:22][C:21]3=[O:27])[C:6]2[C:11](=[O:12])[NH:10][CH:9]=[N:8][C:7]=2[NH:13][C:14]=1[CH3:15])(=[O:3])[CH3:2].F[B-](F)(F)F.[CH2:33]([O+](CC)CC)[CH3:34].CO>ClCCl>[C:1]([C:4]1[CH:5]([C:16]2[CH:17]=[CH:18][CH:19]=[C:20]3[C:25]=2[O:24][C:23]([CH3:26])=[CH:22][C:21]3=[O:27])[C:6]2[C:11]([O:12][CH2:33][CH3:34])=[N:10][CH:9]=[N:8][C:7]=2[NH:13][C:14]=1[CH3:15])(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 887MethanolHCID 2723982Triethyloxonium tetrafluoroborateHCID 1361308496-Acetyl-7-methyl-5-(2-methyl-4-oxo-4H-chromen-8-yl)-5,8-dihydropyrido[2,3-d]pyrimidin-4(3H)-one

生成物 1

HCID 236279908-(6-Acetyl-4-ethoxy-7-methyl-5,8-dihydropyrido[2,3-d]pyrimidin-5-yl)-2-methyl-4H-chromen-4-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

140 mg (0.38 mmol) of 6-acetyl-7-methyl-5-(2-methyl-4-oxo-4H-chromen-8-yl)-5,8-dihydropyrido[2,3-d]pyrimidin-4(3H)-one are suspended under an argon atmosphere in dichloromethane (7 ml), 219 mg (1.15 mmol) of triethyloxonium tetrafluoroborate are added, and the mixture is stirred at RT for 12 h. The reaction mixture is then mixed with methanol and concentrated. The residue is purified by preparative HPLC to result in 9 mg (6% of theory) of the title compound are obtained as a white solid.

後処理

  1. concentrationconcentrated
  2. customThe residue is purified by preparative HPLC

出典と根拠

ORDレコード
ord-66b20ada06bd4533b5f7e3c2bd041e20
出典データセット
uspto-grants-2013_03
特許番号
US08399471B2

反応ノート

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