HCID 20161424、化合物 → HCID 13219227、化合物

HRID 615183ノート

反応式

HRID 615183 の反応式
[C:1]([C:4]1[CH:9]([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([N+:16]([O-:18])=[O:17])[CH:11]=2)[C:8]([C:19]([O:21][CH2:22][CH2:23][C:24]#[N:25])=[O:20])=[C:7]([CH3:26])[NH:6][C:5]=1[CH3:27])(=[O:3])[CH3:2].Cl([O-])(=O)(=O)=O.[Li+]>C(#N)C.[Pt]>[C:1]([C:4]1[C:5]([CH3:27])=[N:6][C:7]([CH3:26])=[C:8]([C:19]([O:21][CH2:22][CH2:23][C:24]#[N:25])=[O:20])[C:9]=1[C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([N+:16]([O-:18])=[O:17])[CH:11]=1)(=[O:3])[CH3:2]

参加物

5

反応物 2

HCID 20161424HCID 20161424、化合物HCID 23665649Lithium perchlorate

生成物 1

HCID 13219227HCID 13219227、化合物

試薬・触媒・溶媒 2

HCID 23939Platinum触媒HCID 6342Acetonitrile溶媒

実験手順

A solution of 10 g (27 mmols) of 2-cyanoethyl 3-acetyl-1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)-pyridine-5-carboxylate in an electrolyte of 5 g of lithium perchlorate in 250 ml of acetonitrile was electrolyzed on a platinum anode at an electrode potential of +1.2 V vs. SCE. After passing through 2 Faraday equivalents, the electrolysis was stopped, the anolyte was evaporated in vacuo, the residue was taken up in a sodium bicarbonate solution and extracted several times with methylene chloride. The organic extracts were washed with water, dried over sodium sulphate and then evaporated in vacuo. The resulting oil crystallized completely, and the solid product was thoroughly stirred in petroleum ether, filtered off with suction and dried, melting point 85° C., yield: 7.5 g (75%).

後処理

  1. customthe anolyte was evaporated in vacuo
  2. extractionextracted several times with methylene chloride
  3. washThe organic extracts were washed with water
  4. dry with materialdried over sodium sulphate
  5. customevaporated in vacuo
  6. customThe resulting oil crystallized completely
  7. filtrationfiltered off with suction
  8. customdried

出典と根拠

ORDレコード
ord-93b8139e47334427870275bccc4bb5f4
出典データセット
uspto-grants-1985_02
特許番号
US04497821

反応ノート

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