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Hydroxyamine hydrochloride → 1-(2,6-Dihydroxyphenyl)-2-methyl-1-propanone oxime

HRID 527533
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HRID 527533 반응식
[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([OH:8])[C:3]=1[C:9](=O)[CH:10]([CH3:12])[CH3:11].Cl.[NH2:15][OH:16]>N1C=CC=CC=1>[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([OH:8])[C:3]=1[C:9](=[N:15][OH:16])[CH:10]([CH3:12])[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochloride2회HCID 134833211-(2,6-Dihydroxyphenyl)-2-methyl-1-propanone2회

생성물 1

HCID 1363786541-(2,6-Dihydroxyphenyl)-2-methyl-1-propanone oxime수율 82.1%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

1-(2,6-dihydroxyphenyl)-2-methyl-1-propanone (Intermediate 37, 416 mg) was dissolved in pyridine (2.0 ml) and hydroxylamine hydrochloride (209 mg, 3.0 mmol) was added. The reaction mixture was then stirred at room temperature overnight. After night, additional hydroxylamine hydrochloride (64 mg, 0.92 mmol) was added and the mixture was heated at 100° C. for 3 hours. After removal of the volatiles, the crude was treated with water and extracted with ethyl acetate. The gathered organic layers were dried over sodium sulphate, filtered and evaporated to afford the title compound (370 mg).

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후처리

  1. waitAfter night
  2. temperaturethe mixture was heated at 100° C. for 3 hours
  3. customAfter removal of the volatiles
  4. additionthe crude was treated with water
  5. extractionextracted with ethyl acetate
  6. dry with materialThe gathered organic layers were dried over sodium sulphate
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-14d6092fb08e4a45b5222e0f7b9b2715
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09346790B2

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