O-Methylhydroxylamine hydrochloride → HCID 136127060、化合物

HRID 432054ノート

反応式

HRID 432054 の反応式
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]

参加物

6

反応物 4

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 135424589methyl E-2-(2-hydroxyphenyl)-2-methoxyimino-acetateHCID 135703866HCID 135703866、化合物HCID 178516824HCID 178516824、化合物

生成物 1

HCID 136127060HCID 136127060、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4315cc39b10b4d7ea0f723b6ad7ee611
出典データセット
uspto-grants-2003_12
特許番号
US06660872B1

反応ノート

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