Triphenylphosphine → ((5,8-Dimethyl-[1,2,4]triazolo[1,5-a]pyrazin-2-yl)methyl)triphenylphosphonium chloride

HRID 1054926노트

반응식

HRID 1054926 반응식
[Cl:1][CH2:2][C:3]1[N:13]=[C:6]2[C:7]([CH3:12])=[N:8][CH:9]=[C:10]([CH3:11])[N:5]2[N:4]=1.[C:14]1([P:20]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>C(#N)C>[Cl-:1].[CH3:11][C:10]1[N:5]2[N:4]=[C:3]([CH2:2][P+:20]([C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=3)[N:13]=[C:6]2[C:7]([CH3:12])=[N:8][CH:9]=1

참가 물질

4

반응물 2

HCID 11776TriphenylphosphineHCID 591512352-(Chloromethyl)-5,8-dimethyl-[1,2,4]triazolo[1,5-a]pyrazine

생성물 1

HCID 86665503((5,8-Dimethyl-[1,2,4]triazolo[1,5-a]pyrazin-2-yl)methyl)triphenylphosphonium chloride수율 110.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 2-(chloromethyl)-5,8-dimethyl-[1,2,4]triazolo[1,5-a]pyrazine (prepared as described in WO2009152825) (500 mg, 2.54 mmol, Eq: 1.00) and triphenylphosphine (667 mg, 2.54 mmol, Eq: 1.00) in acetonitrile (24.9 ml) was refluxed for 18 hours under argon atmosphere. The solvent was evaporated the light pink solid was triturated with ether, the solid was filtered off, washed with ether and dried in vacuo affording (5,8-dimethyl-[1,2,4]triazolo[1,5-a]pyrazin-2-ylmethyl)-triphenyl-phosphonium chloride (1.292 g, 72.5%) as a light pink solid. MS-Cl: m/e=423 (M+H+)

후처리

  1. temperaturewas refluxed for 18 hours under argon atmosphere
  2. customThe solvent was evaporated the light pink solid
  3. customwas triturated with ether
  4. filtrationthe solid was filtered off
  5. washwashed with ether
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-077386b0b00747758c6247a3e03f40d5
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394311B2

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