2-Amino-3-methylpyridine → HCID 20145010, 화합물

HRID 648576노트

반응식

HRID 648576 반응식
Br.[NH2:2][C:3]1[S:4][C:5]([C:9](=O)[CH2:10]Br)=[C:6]([CH3:8])[N:7]=1.[NH2:13][C:14]1[C:19]([CH3:20])=[CH:18][CH:17]=[CH:16][N:15]=1>CC(N(C)C)=O>[NH2:2][C:3]1[S:4][C:5]([C:9]2[N:13]=[C:14]3[C:19]([CH3:20])=[CH:18][CH:17]=[CH:16][N:15]3[CH:10]=2)=[C:6]([CH3:8])[N:7]=1

참가 물질

4

반응물 2

HCID 153472-Amino-3-methylpyridineHCID 20145033HCID 20145033, 화합물

생성물 1

HCID 20145010HCID 20145010, 화합물수율 21.8%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

A solution of 2-amino-4-methyl-5-(2-bromoacetyl)thiazole hydrobromide (9.5 g) and 2-amino-3-methylpyridine (9.7 g) in dimethylacetamide (100 ml) was heated at 85° C. to 88° C. for 5 hours and the reaction mixture was evaporated in vacuo. To the residue was added water and the resulting mixture was acidified to pH 0.8 with 10% hydrochloric acid. The acidified solution was treated with charcoal and filtered. The filtrate was washed with ethyl acetate. The aqueous solution was adjusted to pH 9.0 with aqueous potassium carbonate and extracted with ethyl acetate. The extract was dried over magnesium sulfate and evaporated in vacuo. The residue was recrystallized from a mixture of ethyl acetate and tetrahydrofuran to give 2-(2-amino-4-methyl-5-thiazolyl)-8-methylimidazo[1,2-a]pyridine (1.6 g). mp 226° C. (dec.).

후처리

  1. customthe reaction mixture was evaporated in vacuo
  2. additionTo the residue was added water
  3. additionThe acidified solution was treated with charcoal
  4. filtrationfiltered
  5. washThe filtrate was washed with ethyl acetate
  6. extractionextracted with ethyl acetate
  7. dry with materialThe extract was dried over magnesium sulfate
  8. customevaporated in vacuo
  9. customThe residue was recrystallized from a mixture of ethyl acetate and tetrahydrofuran

출처 및 근거

ORD 기록
ord-6200c0e6291044589e2c2f8d932d110d
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04735957

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