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Methanol → HCID 18326242, 화합물

HRID 1250438
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HRID 1250438 반응식
[Cl:1][C:2]1[C:7](I)=[CH:6][C:5]([C:9]2[C:13]([CH3:14])=[C:12]([C:15]#[N:16])[N:11]([CH3:17])[N:10]=2)=[C:4]([F:18])[CH:3]=1.[CH3:19][OH:20].[C]=[O:22].C(N([CH2:28][CH3:29])CC)C>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>[Cl:1][C:2]1[C:7]([C:19]([O:22][CH2:28][CH3:29])=[O:20])=[CH:6][C:5]([C:9]2[C:13]([CH3:14])=[C:12]([C:15]#[N:16])[N:11]([CH3:17])[N:10]=2)=[C:4]([F:18])[CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 8471TriethylamineHCID 18326232HCID 18326232, 화합물HCID 178418416HCID 178418416, 화합물

생성물 1

HCID 18326242HCID 18326242, 화합물

시약·촉매·용매 1

HCID 178418476HCID 178418476, 화합물촉매

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온도
100 °C

실험 절차

5.2 g of 3-(4-chloro-2-fluoro-5-iodophenyl)-4-methyl-5-cyano-1-methyl-[1H]-pyrazole (Example H8), 60 ml of methanol, 2.8 g of triethylamine and 0.4 g of bis(triphenylphosphine)palladium(II) dichloride (PdCl2(PPh3)2) are placed into a 100 ml pressurized container and stirred for 16 hours at a temperature of 100° C. and a carbon monoxide pressure of 10 megapascal (Mpa). The solvent is subsequently evaporated and the crude product which remains is purified over a silica gel column (eluent: ethyl acetate/hexane 1/5). This gives 3.1 g (69.3% of theory) of the desired product.

후처리

  1. customThe solvent is subsequently evaporated
  2. customthe crude product which remains is purified over a silica gel column (eluent: ethyl acetate/hexane 1/5)

출처 및 근거

ORD 기록
ord-aad0531215d84836ba9ef4c1ca22ba7a
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06339046B1

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