Lithium Hydroxide → 2-(3-Hydroxybutan-2-ylamino)thiazole-4-carboxylic acid

HRID 872659

反応式

HRID 872659 の反応式
[OH:1][CH:2]([CH3:15])[CH:3]([NH:5][C:6]1[S:7][CH:8]=[C:9]([C:11]([O:13]C)=[O:12])[N:10]=1)[CH3:4].[OH-].[Li+]>C1COCC1.O>[OH:1][CH:2]([CH3:15])[CH:3]([NH:5][C:6]1[S:7][CH:8]=[C:9]([C:11]([OH:13])=[O:12])[N:10]=1)[CH3:4]

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 87294675Methyl 2-(3-hydroxybutan-2-ylamino)thiazole-4-carboxylate

生成物 1

HCID 866702512-(3-Hydroxybutan-2-ylamino)thiazole-4-carboxylic acid

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

Methyl 2-(3-hydroxybutan-2-ylamino)thiazole-4-carboxylate (1.092 g, 4.75 mmol) was dissolved in THF/water (9:1) mixture and 1M lithium hydroxide (9.49 ml, 9.49 mmol) was added slowly. The reaction mixture was stirred at RT for 1 h and evaporated to dryness. DCM and water was added and pH was adjusted to 2. Acidic water phase was washed twice with DCM and evaporated to dryness. Evaporation residue was dissolved in ethanol, a precipitation was filtered and the filtrate was evaporated to dryness to give a crude product. m/z [216.3+1].

後処理

  1. additionwas added slowly
  2. customevaporated to dryness
  3. additionDCM and water was added
  4. washAcidic water phase was washed twice with DCM
  5. customevaporated to dryness
  6. customEvaporation residue
  7. dissolutionwas dissolved in ethanol
  8. customa precipitation
  9. filtrationwas filtered
  10. customthe filtrate was evaporated to dryness

出典と根拠

ORDレコード
ord-5ca7acb4135b4aa79f642a01fb27cae0
出典データセット
uspto-grants-2015_03
特許番号
US08975254B2

関連ノート

読み込み中…