Sodium Sulfate → 7-Chloro-6-methoxy-1,2-benzoxazole

HRID 652906ノート

反応式

HRID 652906 の反応式
[Cl:1][C:2]1[C:3]([OH:12])=[C:4]([CH:7]=[CH:8][C:9]=1[O:10][CH3:11])[CH:5]=O.[NH2:13]OS(O)(=O)=O.[O-]S([O-])(=O)=O.[Na+].[Na+].C([O-])(O)=O.[Na+]>O>[Cl:1][C:2]1[C:3]2[O:12][N:13]=[CH:5][C:4]=2[CH:7]=[CH:8][C:9]=1[O:10][CH3:11]

参加物

6

反応物 4

HCID 24436Sodium SulfateHCID 76284hydroxylamine-O-sulfonic acidHCID 516892Sodium BicarbonateHCID 133437063-Chloro-4-methoxysalicylaldehyde

生成物 1

HCID 140125047-Chloro-6-methoxy-1,2-benzoxazole

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

3-chloro-2-hydroxy-4-methoxybenzaldehyde (1.48 g) is suspended in 15 ml of H2O and hydroxylamine-O-sulfonic acid (1.08 g) is added, along with 0.1 g of Na2SO4. After three hours an additional 15 ml of H2O is added. After a total of four hours the reaction mixture is treated with 8% NaHCO3 solution and then extracted into ether. Evaporation and trituration with hexane gives a solid product. Recrystallization from toluene/hexane gives 7-chloro-6-methoxy-1,2-benzisoxazole, mp 115°-118° C.

後処理

  1. extractionextracted into ether
  2. customEvaporation and trituration with hexane
  3. customgives a solid product
  4. customRecrystallization from toluene/hexane

出典と根拠

ORDレコード
ord-36f39b4a82544935ab5750236bab2c0e
出典データセット
uspto-grants-1987_06
特許番号
US04673746

反応ノート

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