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Water → HCID 69590004, 화합물

HRID 890164
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HRID 890164 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]2[C:13]([C:14]([O:16][CH2:17][CH:18]=[CH2:19])=[O:15])=[C:12]([CH3:20])[NH:11][C:10]([CH3:21])=[C:9]2[C:22]([O:24][CH2:25][CH2:26][C:27]#[N:28])=[O:23])[CH:5]=[CH:6][CH:7]=1.I[C:30]1[CH:42]=[CH:41][C:33]([C:34]([O:36][CH2:37][CH2:38][C:39]#[N:40])=[O:35])=[CH:32][CH:31]=1.C(N(CC)CC)C.O>CN(C=O)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]2[C:13]([C:14]([O:16][CH2:17][CH:18]=[CH:19][C:30]3[CH:31]=[CH:32][C:33]([C:34]([O:36][CH2:37][CH2:38][C:39]#[N:40])=[O:35])=[CH:41][CH:42]=3)=[O:15])=[C:12]([CH3:20])[NH:11][C:10]([CH3:21])=[C:9]2[C:22]([O:24][CH2:25][CH2:26][C:27]#[N:28])=[O:23])[CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 222504052-Cyanoethyl 4-iodobenzoateHCID 69590171HCID 69590171, 화합물

생성물 1

HCID 69590004HCID 69590004, 화합물

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매
HCID 6228
Dimethylformamide
용매

실험 절차

307 mg (0.77 mmol) of 5-(2-propene-1-yl) 3-(2-cyanoethyl) 4-(3-chlorophenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate, 278 mg (0.92 mmol) of 2-cyanoethyl 4-iodobenzoate, 19 mg(0.08 mmol) of palladium acetate and 0.14 ml (1.0 mmol) of triethylamine were heated at 100° C. under stirring in 5 ml of DMF overnight. Water was added to the reaction mixture. After the extraction with ethyl acetate, the organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by the silica gel chromatography (hexane/ethyl acetate=2/1) to obtain the title compound.

후처리

  1. extractionAfter the extraction with ethyl acetate
  2. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by the silica gel chromatography (hexane/ethyl acetate=2/1)

출처 및 근거

ORD 기록
ord-74f5db127eaa42898f49e40d60a784b8
출처 데이터셋
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06995179B2

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