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Water → (+)-2-{7-[4-(5-methyl-[1,2,4]-oxadiazole-3-yl)phenyl]-[1,4]-oxazepane-4-yl}-3-methyl-6-pyrimidin-4-yl-3H-pyrimidin-4-one

HRID 515482
ノート
印刷プレビュー

反応式

HRID 515482 の反応式
Cl.[CH3:2][C:3]1[O:7][N:6]=[C:5]([C:8]2[CH:13]=[CH:12][C:11]([CH:14]3[O:20][CH2:19][CH2:18][NH:17][CH2:16][CH2:15]3)=[CH:10][CH:9]=2)[N:4]=1.Cl[C:22]1[N:27]([CH3:28])[C:26](=[O:29])[CH:25]=[C:24]([C:30]2[CH:35]=[CH:34][N:33]=[CH:32][N:31]=2)[N:23]=1.C(N(CC)CC)C.O>C(Cl)(Cl)Cl>[CH3:2][C:3]1[O:7][N:6]=[C:5]([C:8]2[CH:9]=[CH:10][C:11]([CH:14]3[O:20][CH2:19][CH2:18][N:17]([C:22]4[N:27]([CH3:28])[C:26](=[O:29])[CH:25]=[C:24]([C:30]5[CH:35]=[CH:34][N:33]=[CH:32][N:31]=5)[N:23]=4)[CH2:16][CH2:15]3)=[CH:12][CH:13]=2)[N:4]=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 962WaterHCID 8471TriethylamineHCID 179544602-Chloro-3-methyl-6-(pyrimidin-4-YL)pyrimidin-4-oneHCID 667185737-[4-(5-Methyl-[1,2,4]oxadiazol-3-yl)-phenyl]-[1,4]oxazepane hydrochloride

生成物 1

HCID 67281171(+)-2-{7-[4-(5-methyl-[1,2,4]-oxadiazole-3-yl)phenyl]-[1,4]-oxazepane-4-yl}-3-methyl-6-pyrimidin-4-yl-3H-pyrimidin-4-one収率 50%

試薬・触媒・溶媒

1
HCID 6212Chloroform溶媒

実験手順

To a slurry of optically active 7-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)-phenyl]-[1,4]oxazepane hydrochloride (0.12 g, 0.41 mmol) and 2-chloro-3-methyl-6-(pyrimidin-4-yl)-3H-pyrimidin-4-one (0.09 g, 0.38 mmol) was added triethylamine (0.21 mL, 1.5 mmol) at room temperature. The mixture was stirred for 20 hours and poured into water. Extractive workup with chloroform was performed and the organic phase was dried over sodium sulfate. Concentration followed by purification of the residue by flash column chromatography on silica gel (chloroform/methanol=100/0 to 90/10 as eluants) yielded (+)-2-{7-[4-(5-methyl-[1,2,4]-oxadiazole-3-yl)phenyl]-[1,4]-oxazepane-4-yl}-3-methyl-6-pyrimidin-4-yl-3H-pyrimidin-4-one (A100) (0.09 g, 0.19 mmol, 50%) as yellowish solid.

後処理

  1. dry with materialthe organic phase was dried over sodium sulfate
  2. concentrationConcentration
  3. customfollowed by purification of the residue by flash column chromatography on silica gel (chloroform/methanol=100/0 to 90/10 as eluants)

出典と根拠

ORDレコード
ord-fb84f6e221a341afbb5af10603562120
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09108957B2

反応ノート

読み込み中…

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