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

HRID 872659

반응식

HRID 872659 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

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].

후처리

  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

출처 및 근거

ORD 기록
ord-5ca7acb4135b4aa79f642a01fb27cae0
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08975254B2

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