Ammonium Hydroxide → HCID 9859347, 화합물

HRID 1614178노트

반응식

HRID 1614178 반응식
[NH2:1][C:2]1[O:3][C:4]([C:11](=O)[C:12]([CH3:15])([CH3:14])[CH3:13])=[C:5]([C:7]([CH3:10])([CH3:9])[CH3:8])[N:6]=1.[OH-].[NH4+:18]>C(O)(C)(C)C>[NH2:1][C:2]1[N:18]=[C:11]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:4]([OH:3])=[C:5]([C:7]([CH3:10])([CH3:9])[CH3:8])[N:6]=1

참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 19101100HCID 19101100, 화합물

생성물 1

HCID 9859347HCID 9859347, 화합물수율 34%

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

A solution of 1-[2-amino-4-(1,1-dimethylethyl)-5-oxazolyl]-2,2-dimethyl-1-propanone (15 g) in t-butanol (80 mL) and concentrated ammonium hydroxide (80 mL) is heated at 180° C. for 60 hours in a steel bomb. The reaction mixture is cooled and concentrated to half its volume on the rotovap. The product is extracted into ether (3×250 mL). The ether extract is dried (MgSO4) and evaporated. The residue is purified by flash chromatography (silica, 20% EtOAc/hexane) to give pure 2-amino-4,6-bis(1,1-dimethylethyl)-5-hydroxypyrimidine (4.5 g, 34%) which crystallizes from cold hexane; mp 92°-93° C.

후처리

  1. temperatureThe reaction mixture is cooled
  2. concentrationconcentrated to half its volume on the rotovap
  3. extractionThe product is extracted into ether (3×250 mL)
  4. extractionThe ether extract
  5. dry with materialis dried (MgSO4)
  6. customevaporated
  7. customThe residue is purified by flash chromatography (silica, 20% EtOAc/hexane)

출처 및 근거

ORD 기록
ord-6884affa1071459aa79ebc6759fa6261
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05196431

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