Sodium Hydroxide → 2-(4,6-Dimethyl-5-nitropyrimidine-2-ylamino)acetic acid

HRID 1749266ノート

反応式

HRID 1749266 の反応式
[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([CH3:11])[N:5]=[C:4]([NH:12][CH2:13][C:14]([O:16]CC)=[O:15])[N:3]=1.[OH-].[Na+]>O1CCOCC1>[CH3:11][C:6]1[C:7]([N+:8]([O-:10])=[O:9])=[C:2]([CH3:1])[N:3]=[C:4]([NH:12][CH2:13][C:14]([OH:16])=[O:15])[N:5]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 25120135Ethyl 2-(4,6-dimethyl-5-nitropyrimidine-2-ylamino)acetate

生成物 1

HCID 593361022-(4,6-Dimethyl-5-nitropyrimidine-2-ylamino)acetic acid収率 75%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
25 °C

実験手順

Compound 10 (80 mg) was suspended in 1,4-dioxane (1.5 mL) and a 2N aqueous sodium hydroxide solution (1.5 mL) was added at room temperature (20 to 30° C.). The mixture was stirred at room temperature (20 to 30° C.) for 8 hours. Subsequently, the mixture was washed with diethyl ether. While the reaction mixture was cooled, a 2N aqueous HCl solution was added portionwise to neutralize the mixture to a pH of 3. The mixture was extracted twice with chloroform and the organic layer was concentrated under reduced pressure to give 52 mg (75% yield) of the desired product as a pale yellow amorphous.

後処理

  1. washSubsequently, the mixture was washed with diethyl ether
  2. temperatureWhile the reaction mixture was cooled
  3. additiona 2N aqueous HCl solution was added portionwise
  4. extractionThe mixture was extracted twice with chloroform
  5. concentrationthe organic layer was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-66d5b3d38c6441469237eff69c018d3d
出典データセット
uspto-grants-2015_10
特許番号
US09156817B2

反応ノート

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