Hydrochloric Acid → HCID 178502623、化合物

HRID 612806ノート

反応式

HRID 612806 の反応式
CC(C)([O-])C.[K+].[CH3:7][O:8][N:9]=[C:10]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[O:12][CH2:11]1.[N:19](OC(C)(C)C)=[O:20].Cl>C(O)(C)(C)C>[CH3:7][O:8][N:9]=[C:10]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[O:12][C:11]1=[N:19][OH:20]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10906Tert-Butyl nitriteHCID 23665647Potassium tert-butoxideHCID 54271616benzofuran-3-one O-methyl oxime

生成物 1

HCID 178502623HCID 178502623、化合物収率 47.4%

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒2 回

実験手順

3.92 g (0.035 mol) of potassium tert-butoxide are dissolved in 40 ml of tert-butanol. A solution of 5.7 g (0.035 mol) of benzofuran-3-one O-methyl-oxime and 7.2 g (0.07 mol) of tert-butyl nitrite in 10 ml of tert-butanol is added to this solution. The mixture is stirred without cooling for two hours and then admixed with 20 ml of 2N aqueous hydrochloric acid. The crystalline product is filtered off, washed repeatedly with water and dried in a desiccator. 3.19 g (47.1% of theory) of benzofuran-2,3-dione 3-(O-methyl-oxime) 2-oxime are obtained as a mixture of two stereoisomers comprising 86.33% of isomer A and 12.98% of isomer B (HPLC).

後処理

  1. temperaturewithout cooling for two hours
  2. filtrationThe crystalline product is filtered off
  3. washwashed repeatedly with water
  4. customdried in a desiccator

出典と根拠

ORDレコード
ord-c8902eb2e08d49ddacccd338e7b6ef37
出典データセット
uspto-grants-1999_12
特許番号
US06005104

反応ノート

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