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Pyridine → Ethyl 2-(2,4,5-trichlorophenyl)oxycarbonyloxyimino-2-cyanoacetate

HRID 1283760
ノート
印刷プレビュー

反応式

HRID 1283760 の反応式
Cl[C:2]([O:4][N:5]=[C:6]([C:12]#[N:13])[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:3].[Cl:14][C:15]1[CH:20]=[C:19]([Cl:21])[C:18]([Cl:22])=[CH:17][C:16]=1[OH:23].N1C=CC=CC=1>C1C=CC=CC=1>[Cl:14][C:15]1[CH:20]=[C:19]([Cl:21])[C:18]([Cl:22])=[CH:17][C:16]=1[O:23][C:2]([O:4][N:5]=[C:6]([C:12]#[N:13])[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 72712,4,5-TrichlorophenolHCID 53929971Ethyl 2-chlorocarbonyloxyimino-2-cyanoacetate

生成物 1

HCID 54542381Ethyl 2-(2,4,5-trichlorophenyl)oxycarbonyloxyimino-2-cyanoacetate収率 65.7%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To a solution of ethyl 2-chlorocarbonyloxyimino-2-cyanoacetate (0.05 mol) prepared as in Example 11 (1), a solution of 2,4,5-trichlorophenol (9.9 g) and pyridine (3.9 g) in benzene (50 ml) is dropwise added under cooling with icewater. The resulting mixture is stirred for 1 hour and allowed to stand over night. The reaction mixture is washed with water, dried and concentrated. The residue is admixed with petroleum ether and filtered to collect crystals, which is dried and recrystallized from a benzene-petroleum ether mixture to give ethyl 2-(2,4,5-trichlorophenyl)oxycarbonyloxyimino-2-cyanoacetate (12.0 g). M.P. 101 to 103°C.

後処理

  1. temperatureunder cooling with icewater
  2. waitto stand over night
  3. washThe reaction mixture is washed with water
  4. customdried
  5. concentrationconcentrated
  6. filtrationfiltered
  7. customto collect crystals, which
  8. customis dried
  9. customrecrystallized from a benzene-petroleum ether mixture

出典と根拠

ORDレコード
ord-f7a2a26cccc8422891c3cb340c4cd9f2
出典データセット
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03976635

反応ノート

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