Pyridine → 2-benzyloxyacetophenone O-methyloxime

HRID 892935ノート

反応式

HRID 892935 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 541941012-benzyloxyacetophenone O-methyloxime収率 97.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7a3a4126edcb4428aa2016ce5213fa63
出典データセット
uspto-grants-1992_06
特許番号
US05120853

反応ノート

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