Hydrochloric Acid → HCID 178502623, 화합물

HRID 612806노트

반응식

HRID 612806 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 178502623HCID 178502623, 화합물수율 47.4%

시약·촉매·용매 1

HCID 6386tert-Butanol용매2회

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-c8902eb2e08d49ddacccd338e7b6ef37
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06005104

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