HCID 20161424, 화합물 → HCID 13219227, 화합물

HRID 615183노트

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HRID 615183 반응식
[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]

참가 물질

5

반응물 2

HCID 20161424HCID 20161424, 화합물HCID 23665649Lithium perchlorate

생성물 1

HCID 13219227HCID 13219227, 화합물

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 6342Acetonitrile용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-93b8139e47334427870275bccc4bb5f4
출처 데이터셋
uspto-grants-1985_02
특허 번호
US04497821

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