2-Amino-3-methylpyridine → HCID 20145010、化合物

HRID 1905995ノート

反応式

HRID 1905995 の反応式
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

参加物

4

反応物 2

HCID 153472-Amino-3-methylpyridineHCID 20145033HCID 20145033、化合物

生成物 1

HCID 20145010HCID 20145010、化合物収率 21.8%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

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.)

後処理

  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

出典と根拠

ORDレコード
ord-d556ae71631446d4adc483c30e4fbf05
出典データセット
uspto-grants-1987_03
特許番号
US04649146

反応ノート

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