Lithium hydroxide, monohydrate → Lithium 2-thioxo-2,3-dihydrobenzoxazole-4-carboxylate

HRID 249863ノート

反応式

HRID 249863 の反応式
[S:1]=[C:2]1[NH:6][C:5]2=[C:7]([C:11]([O:13]C)=[O:12])[CH:8]=[CH:9][CH:10]=[C:4]2[O:3]1.O.[OH-].[Li+:17]>C1COCC1.O>[S:1]=[C:2]1[NH:6][C:5]2=[C:7]([C:11]([O-:13])=[O:12])[CH:8]=[CH:9][CH:10]=[C:4]2[O:3]1.[Li+:17]

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 22272869Methyl 2-thioxo-2,3-dihydrobenzoxazole-4-carboxylate

生成物 1

HCID 86623720Lithium 2-thioxo-2,3-dihydrobenzoxazole-4-carboxylate収率 96.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
75 °C

実験手順

To a solution of methyl 2-thioxo-2,3-dihydrobenzoxazole-4-carboxylate (150 mg, 0.72 mmol) in THF (6 mL) was added a solution of lithium hydroxide monohydrate (45.1 mg, 1.08 mmol) in H2O (3 mL). The reaction mixture was heated to 75° C. with stirring for 3 days, cooled down to room temperature and concentrated under reduced pressure to afford the lithium 2-thioxo-2,3-dihydrobenzoxazole-4-carboxylate (135 mg, 96.5%) as a yellow solid. MS consistent

後処理

  1. temperaturecooled down to room temperature
  2. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-594f69d80b204df6a9ebf4a3bc0545bc
出典データセット
uspto-grants-2011_01
特許番号
US07863271B2

反応ノート

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