Triphenylphosphine → Chloride

HRID 2175357ノート

反応式

HRID 2175357 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>[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.[Cl-:1]

参加物

5

反応物 2

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

生成物 2

HCID 312ChlorideHCID 59151223(5,8-Dimethyl-[1,2,4]triazolo[1,5-a]pyrazin-2-ylmethyl)-triphenyl-phosphonium

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 2-chloromethyl-5,8-dimethyl-[1,2,4]triazolo[1,5-a]pyrazine (1.351 g, 6.87 mmol) and triphenylphosphine (1.80 g, 6.87 mmol) in acetonitrile 150 mL was heated at reflux for 12 h. The solvents were removed in vacuo and the residue slurried in ether, filtered and dried to yield (5,8-Dimethyl-[1,2,4]triazolo[1,5-a]pyrazin-2-ylmethyl)-triphenyl-phosphonium, chloride as an off white solid (2.412 g, 74.9%). LC-MS: m/z=423.2 ([M-Cl]*), tR=0.86 minutes, method A.

後処理

  1. temperatureat reflux for 12 h
  2. customThe solvents were removed in vacuo
  3. filtrationfiltered
  4. customdried

出典と根拠

ORDレコード
ord-1902a3f0ce94462490087a2f7f3517da
出典データセット
uspto-grants-2015_06
特許番号
US09062060B2

反応ノート

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