Pyridine → 2-benzyloxyacetophenone O-methyloxime

HRID 1085995노트

반응식

HRID 1085995 반응식
N1C=CC=CC=1.[CH2:7]([O:14][CH2:15][C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.Cl.[CH3:25][O:26][NH2:27]>O>[CH3:25][O:26][N:27]=[C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH2:15][O:14][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 521874O-Methylhydroxylamine hydrochlorideHCID 112531252-(Benzyloxy)-1-phenylethan-1-one

생성물 1

HCID 541941012-benzyloxyacetophenone O-methyloxime수율 97.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 50 ml of pyridine were added 0.0434 mole (9.77 g) of 2-benzyloxyacetophenone prepared in the first and second paragraphs in Referential Example 1 (Table 1, No. 1) and 4.35 g (0.0521 mole) of O-methylhydroxylamine hydrochloride. The mixture was stirred at room temperature for 2 hours and then at 100° C. for 1 hour. The reaction liquid was cooled down to room temperature, 300 ml of water was added thereto, and the oil layer was separated off. The aqueous layer was extracted with chloroform and the extract was combined with said oil layer, washed with water, dried and distilled under reduced pressure to obtain 10.77 g of 2-benzyloxyacetophenone O-methyloxime.

후처리

  1. customprepared in the first and second paragraphs in Referential Example 1 (Table 1
  2. waitat 100° C. for 1 hour
  3. customThe reaction liquid
  4. temperaturewas cooled down to room temperature
  5. customthe oil layer was separated off
  6. extractionThe aqueous layer was extracted with chloroform
  7. washwashed with water
  8. customdried
  9. distillationdistilled under reduced pressure

출처 및 근거

ORD 기록
ord-fbc2bf8017d44237a15500a0c66576a7
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05011989

반응 노트

불러오는 중…