Triphenylphosphine → Chloride

HRID 2175357노트

반응식

HRID 2175357 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>[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]

참가 물질

5

반응물 2

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

생성물 2

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-1902a3f0ce94462490087a2f7f3517da
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09062060B2

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