Lithium Hydroxide → HCID 57500673、化合物

HRID 2174919ノート

反応式

HRID 2174919 の反応式
[O:1]=[C:2]1[C:11]2[N:12]=[CH:13][S:14][C:10]=2[C:9]2[CH:8]=[CH:7][C:6]([C:15]([O:17]C)=[O:16])=[CH:5][C:4]=2[NH:3]1.[Li+].[OH-].C1COCC1.[OH-].[Na+]>O.CO>[O:1]=[C:2]1[C:11]2[N:12]=[CH:13][S:14][C:10]=2[C:9]2[CH:8]=[CH:7][C:6]([C:15]([OH:17])=[O:16])=[CH:5][C:4]=2[NH:3]1

参加物

7

反応物 4

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 57500672HCID 57500672、化合物

生成物 1

HCID 57500673HCID 57500673、化合物収率 2.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

Methyl 4-oxo-4,5-dihydrothiazolo[4,5-c]quinoline-7-carboxylate (35 mg, 0.12 mmol) and LiOH (60 mg, 0.83 mmol) were stirred in a (1:1:1, v:v:v) mixture of THF, MeOH and water (0.6 ml) for 2 hours. 6N aqueous NaOH was added and the solution filtered through celite. The solution was acidified and the resulting solid filtered. Preparative HPLC purification and genevac evaporation provided 4-oxo-4,5-dihydrothiazolo[4,5-c]quinoline-7-carboxylic acid as a white solid (0.8 mg). LCMS (ES): 95% pure, m/z 247 [M+1]+.

後処理

  1. filtrationthe solution filtered through celite
  2. filtrationthe resulting solid filtered
  3. customPreparative HPLC purification and genevac evaporation

出典と根拠

ORDレコード
ord-635604427ced4c70ba0d8e328774afc1
出典データセット
uspto-grants-2015_06
特許番号
US09062043B2

反応ノート

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