Triphenylphosphine → HCID 86643670, 화합물

HRID 215855노트

반응식

HRID 215855 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(OC(=O)O[C@H:25]1[CH2:29][C@@H:28]([N:30]2[CH:38]=[N:37][C:36]3[C:31]2=[N:32][C:33]([Cl:40])=[N:34][C:35]=3[Cl:39])[CH:27]=[CH:26]1)C.[CH2:42]([C:44]1[CH:48]=[N:47][NH:46][N:45]=1)[CH3:43]>C1COCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Cl:40][C:33]1[N:32]=[C:31]2[C:36]([N:37]=[CH:38][N:30]2[C@@H:28]2[CH2:29][C@H:25]([N:47]3[CH:48]=[C:44]([CH2:42][CH3:43])[N:45]=[N:46]3)[CH:26]=[CH:27]2)=[C:35]([Cl:39])[N:34]=1

참가 물질

6

반응물 3

HCID 11776TriphenylphosphineHCID 147949874-ethyl-2H-1,2,3-TriazoleHCID 58025019Carbonic acid (1S,4R)-4-(2,6-dichloro-purin-9-yl)-cyclopent-2-enyl ester ethyl ester

생성물 1

HCID 86643670HCID 86643670, 화합물

시약·촉매·용매 2

HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 8028Tetrahydrofuran용매2회

실험 절차

A mixture comprising triphenylphosphine (0.299 g, 0.874 mmol) and Pd2(dba)3 (0.267 g, 0.291 mmol) in dry THF (5 mL) under an inert atmosphere of argon is stirred at RT for 10 minutes. This mixture is then added to a pre-stirring mixture of carbonic acid (1S,4R)-4-(2,6-dichloro-purin-9-yl)-cyclopent-2-enyl ester ethyl ester (Intermediate AA2) (2.00 g, 5.83 mmol) and 4-ethyl-2H-[1,2,3]triazole (0.594 g, 6.12 mmol) in THF (15 mL). The resulting mixture is stirred at RT overnight and then concentrated in vacuo. The crude product is purified by chromatography on silica eluting with 0-50% EtOAc in iso-hexane to afford the title compound as a white solid. (MH+ 350).

후처리

  1. concentrationconcentrated in vacuo
  2. customThe crude product is purified by chromatography on silica eluting with 0-50% EtOAc in iso-hexane

출처 및 근거

ORD 기록
ord-1d4ea045696d4bc38530429a916155ad
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193164B2

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