Lithium Hydroxide → 3,4-Dimethylbenzothiazol-2-one-5-carboxylic acid

HRID 1071908ノート

反応式

HRID 1071908 の反応式
[CH3:1][N:2]1[C:6]2[C:7]([CH3:15])=[C:8]([C:11]([O:13]C)=[O:12])[CH:9]=[CH:10][C:5]=2[S:4][C:3]1=[O:16].[OH-].[Li+]>O1CCCC1.O>[CH3:1][N:2]1[C:6]2[C:7]([CH3:15])=[C:8]([C:11]([OH:13])=[O:12])[CH:9]=[CH:10][C:5]=2[S:4][C:3]1=[O:16]

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 22390078Methyl 3,4-dimethylbenzothiazol-2-one-5-carboxylate

生成物 1

HCID 223900833,4-Dimethylbenzothiazol-2-one-5-carboxylic acid収率 83.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 10.15 g (43 mmol) of methyl 3,4-dimethylbenzo-thiazol-2-one-5-carboxylate in 100 ml of tetrahydrofuran and 100 ml of water was admixed with 2.06 g (86 mmol) of lithium hydroxide. The solution was then heated at reflux for 2 hours. After cooling, the tetrahydrofuran was removed under reduced pressure, the remaining aqueous solution was acidified and the precipitated solid was filtered off with suction and dried. More product was obtained by extracting the mother liquor with ethyl acetate. This gave a total of 8 g (36 mmol, 83% yield) of 3,4-dimethylbenzothiazol-2-one-5-carboxylic acid of m.p. 235° C.-239° C.

後処理

  1. temperatureThe solution was then heated
  2. temperatureat reflux for 2 hours
  3. temperatureAfter cooling
  4. customthe tetrahydrofuran was removed under reduced pressure
  5. filtrationthe precipitated solid was filtered off with suction
  6. customdried
  7. customMore product was obtained
  8. extractionby extracting the mother liquor with ethyl acetate

出典と根拠

ORDレコード
ord-0e5a17ca05fa4c5a8b3ee901968bfa26
出典データセット
uspto-grants-2005_06
特許番号
US06908884B2

反応ノート

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