Hydroxyamine hydrochloride → 5-(Thiophen-2-YL)-1,2-oxazole

HRID 2184794노트

반응식

HRID 2184794 반응식
CN(C)[C:3](=[CH2:11])[C:4]([C:6]1[S:7][CH:8]=[CH:9][CH:10]=1)=[O:5].Cl.[NH2:14]O>CO>[S:7]1[CH:8]=[CH:9][CH:10]=[C:6]1[C:4]1[O:5][N:14]=[CH:11][CH:3]=1

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 22288452beta-Dimethylamino-1-(2-thienyl)-2-propen-1-one

생성물 1

HCID 120499865-(Thiophen-2-YL)-1,2-oxazole수율 97%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of β-dimethylamino-1-(2-thienyl)-2-propen-1-one (1) (18.1 g, 100 mmol) and hydroxylamine hydrochloride (7.0 g, 101 mmol) in anhydrous methanol (100 mL) is refluxed under nitrogen for 2 hrs. The reaction mixture is cooled, concentrated and partitioned between water and dichloromethane. The dichloromethane layer is dried with anhydrous sodium sulfate, filtered and concentrated to yield product (2) as a dark yellow-orange oil (14.7 g, 97 mmol, 97%).

후처리

  1. temperatureis refluxed under nitrogen for 2 hrs
  2. temperatureThe reaction mixture is cooled
  3. concentrationconcentrated
  4. custompartitioned between water and dichloromethane
  5. dry with materialThe dichloromethane layer is dried with anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-336c0b89ef8d4754915d17a80ed200fe
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06399621B1

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