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

HRID 1054926ノート

反応式

HRID 1054926 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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+)

後処理

  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

出典と根拠

ORDレコード
ord-077386b0b00747758c6247a3e03f40d5
出典データセット
uspto-grants-2016_07
特許番号
US09394311B2

反応ノート

読み込み中…