Triethylamine → HCID 73446456, 화합물

HRID 1271040

반응식

HRID 1271040 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]#[CH:9])=[CH:4][CH:3]=1.C(N(CC)CC)C.[Cl:17][C:18]1[C:23](I)=[CH:22][N:21]=[C:20]([N:25]=[CH:26][N:27]([CH:31]([CH3:33])[CH3:32])[CH:28]([CH3:30])[CH3:29])[N:19]=1>C(#N)C.[Cu](I)I.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]#[C:9][C:23]2[C:18]([Cl:17])=[N:19][C:20]([N:25]=[CH:26][N:27]([CH:31]([CH3:33])[CH3:32])[CH:28]([CH3:29])[CH3:30])=[N:21][CH:22]=2)=[CH:4][CH:3]=1

참가 물질

7

반응물 3

HCID 8471TriethylamineHCID 136603Benzene, 1-bromo-4-ethynyl-HCID 734464514-Chloro-2-diisopropylaminomethyleneamino-5-iodopyrimidine

생성물 1

HCID 73446456HCID 73446456, 화합물수율 78.1%

시약·촉매·용매 3

HCID 83717Copper iodide촉매HCID 178418476HCID 178418476, 화합물촉매HCID 6342Acetonitrile용매

실험 절차

A mixture of 0.5 g of 1-bromo-4-ethynylbenzene, 5.0 mL of triethylamine, 0.031 mg of copper iodide, 0.94 g of 4-chloro-2-diisopropylaminomethyleneamino-5-iodopyrimidine and 0.046 g of dichlorobis(triphenyl)phosphine palladium II was magnetically stirred at room temperature for 18 hrs. The mixture was diluted with acetonitrile, filtered and the filtrate evaporated in vacuo. The evaporated filtrate was dissolved in dichloromethane and loaded on a column of silica gel equilibrated in the same solvent. Cuts were monitored by thin layer chromatography. After initial cuts of brown colored eluates, the product subsequently eluted as yellow fractions. Like cuts were pooled and evaporated to give 0.84 g of 5-(4-bromophenylethynyl)-4-chloro-2-diisopropylaminomethyleneaminopyrimidine as a thick amber syrup.

후처리

  1. filtrationfiltered
  2. customthe filtrate evaporated in vacuo
  3. dissolutionThe evaporated filtrate was dissolved in dichloromethane
  4. washAfter initial cuts of brown colored eluates, the product subsequently eluted as yellow fractions
  5. customevaporated

출처 및 근거

ORD 기록
ord-6ec0d97fa2584cd3b1674bb15858e107
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07205297B2

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