Sodium Hydroxide → Tert-butyl [4-(5-methanesulfonyl-7-propoxyoxazolo[5,4-d]pyrimidin-2-yl)-2,6-dimethylphenoxy]acetate

HRID 81503

反応式

HRID 81503 の反応式
[CH3:1][C:2]1[CH:16]=[C:15]([C:17]2[O:18][C:19]3[N:20]=[C:21]([S:30][CH3:31])[N:22]=[C:23]([O:26][CH2:27][CH2:28][CH3:29])[C:24]=3[N:25]=2)[CH:14]=[C:13]([CH3:32])[C:3]=1[O:4][CH2:5][C:6]([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7].ClC1C=CC=C(C(OO)=[O:41])C=1.[OH-:44].[Na+]>ClCCl>[CH3:31][S:30]([C:21]1[N:22]=[C:23]([O:26][CH2:27][CH2:28][CH3:29])[C:24]2[N:25]=[C:17]([C:15]3[CH:16]=[C:2]([CH3:1])[C:3]([O:4][CH2:5][C:6]([O:8][C:9]([CH3:11])([CH3:10])[CH3:12])=[O:7])=[C:13]([CH3:32])[CH:14]=3)[O:18][C:19]=2[N:20]=1)(=[O:41])=[O:44]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 70297m-Chloroperbenzoic acidHCID 86688232HCID 86688232、化合物

生成物 1

HCID 86679896Tert-butyl [4-(5-methanesulfonyl-7-propoxyoxazolo[5,4-d]pyrimidin-2-yl)-2,6-dimethylphenoxy]acetate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

250 mg of tert-butyl [2,6-dimethyl-4-(5-methylsulfanyl-7-propoxyoxazolo[5,4-d]pyrimidin-2-yl)phenoxy]acetate were dissolved in 5 ml of dichloromethane. At 0° C., 268 mg of 3-chlorperbenzoic acid were then added, after which the mixture was stirred at room temperature for 12 h. The mixture was treated with 1 M aqueous sodium hydroxide solution, the layers were then separated and the organic layer was subsequently extracted twice with dichloromethane. The combined organic phases were washed with 10% strength aqueous sodium bisulfite solution, dried over sodium sulfate, filtered and evaporated under reduced pressure. This gave 268 mg of the title compound.

後処理

  1. customthe layers were then separated
  2. extractionthe organic layer was subsequently extracted twice with dichloromethane
  3. washThe combined organic phases were washed with 10% strength aqueous sodium bisulfite solution
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-689997b834d943a48b8a654f0932247a
出典データセット
uspto-grants-2014_09
特許番号
US08846691B2

関連ノート

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