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

HRID 249863

반응식

HRID 249863 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
75 °C

실험 절차

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

후처리

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

출처 및 근거

ORD 기록
ord-594f69d80b204df6a9ebf4a3bc0545bc
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07863271B2

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