Hydrochloric Acid → 2-(6-Bromo-2-methylpyrimidin-4-ylamino)thiazole-5-formic acid

HRID 515256ノート

反応式

HRID 515256 の反応式
[Br:1][C:2]1[N:7]=[C:6]([CH3:8])[N:5]=[C:4]([NH:9][C:10]2[S:11][C:12]([C:15]([O:17]C)=[O:16])=[CH:13][N:14]=2)[CH:3]=1.[OH-].[Na+].Cl>O>[Br:1][C:2]1[N:7]=[C:6]([CH3:8])[N:5]=[C:4]([NH:9][C:10]2[S:11][C:12]([C:15]([OH:17])=[O:16])=[CH:13][N:14]=2)[CH:3]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 49821806Methyl 2-(6-bromo-2-methylpyrimidin-4-ylamino)thiazole-5-formate2 回

生成物 1

HCID 498218842-(6-Bromo-2-methylpyrimidin-4-ylamino)thiazole-5-formic acid収率 78.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Methyl 2-(6-bromo-2-methylpyrimidin-4-ylamino)thiazole-5-formate (Compound 11) (32.9 g, 0.1 mol) was added into a solution of NaOH (8.0 g, 0.2 mol) in water (250 mL) prepared in advance, and reacted by stirring at room temperature overnight. After filtration the filtrate was transferred into reaction flask and pH value was adjusted to 6-6.5 with hydrochloric acid (6N) when the temperature is controlled between 20° C. and 25° C. Grew the grain by stirring for 2 h, and then filtrated and dried to give Compound 12 (21.2 g, yield: 78.3%).

後処理

  1. customprepared in advance
  2. customreacted
  3. filtrationAfter filtration the filtrate
  4. customwas transferred into reaction flask and pH value
  5. customis controlled between 20° C. and 25° C
  6. stirringGrew the grain by stirring for 2 h
  7. filtrationfiltrated
  8. customdried

出典と根拠

ORDレコード
ord-0235a1831eb142f1a0184a149de35a6a
出典データセット
uspto-grants-2015_08
特許番号
US09108954B2

反応ノート

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