O-Methylhydroxylamine hydrochloride → HCID 136127060, 화합물

HRID 432054노트

반응식

HRID 432054 반응식
O1C2C=CC=CC=2C(=O)C1=NO.Cl.CON.[OH:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1/[C:24](=[N:29]\[O:30][CH3:31])/[C:25]([O:27][CH3:28])=[O:26].OC1C=CC=CC=1/C(=N/OC)/C(OC)=O>CO>[OH:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[C:24](=[N:29][O:30][CH3:31])[C:25]([O:27][CH3:28])=[O:26]

참가 물질

6

반응물 4

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 135424589methyl E-2-(2-hydroxyphenyl)-2-methoxyimino-acetateHCID 135703866HCID 135703866, 화합물HCID 178516824HCID 178516824, 화합물

생성물 1

HCID 136127060HCID 136127060, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

8.2 g (0.05 mol) of benzofuran-2,3-dione 2-oxime and 9 g (0.108 mol) of O-methylhydroxylamine hydrochloride in 50 ml of methanol are heated under reflux for 3 hours. The methanol is distilled off under reduced pressure and the residue is mixed with 50 ml of water and extracted with ethyl acetate. The organic phase is dried over sodium sulphate and the solvent is distilled off under reduced pressure, giving 9.88 g of crystal-containing crude product. According to HPLC, the crude product contains 43.7% of methyl E-2-(2-hydroxyphenyl)-2-methoxyimino-acetate of log p=1.48 and 29.4% of methyl Z-2-(2-hydroxyphenyl)-2-methoxyimino-acetate of log p=2.37.

후처리

  1. temperatureunder reflux for 3 hours
  2. distillationThe methanol is distilled off under reduced pressure
  3. additionthe residue is mixed with 50 ml of water
  4. extractionextracted with ethyl acetate
  5. dry with materialThe organic phase is dried over sodium sulphate
  6. distillationthe solvent is distilled off under reduced pressure
  7. customgiving 9.88 g
  8. additionof crystal-containing crude product

출처 및 근거

ORD 기록
ord-4315cc39b10b4d7ea0f723b6ad7ee611
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06660872B1

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