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

HRID 1749266노트

반응식

HRID 1749266 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-66d5b3d38c6441469237eff69c018d3d
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09156817B2

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