Triphenylphosphine → HCID 23076402、化合物

HRID 2221662ノート

反応式

HRID 2221662 の反応式
[ClH:1].[Cl:2][CH2:3][C:4]1[CH:5]=[N:6][N:7]([CH2:9][CH3:10])[CH:8]=1.[C:11]1([P:17]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>C(#N)C>[ClH:2].[Cl-:1].[CH2:9]([N:7]1[CH:8]=[C:4]([CH2:3][P+:17]([C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:5]=[N:6]1)[CH3:10]

参加物

4

反応物 2

HCID 11776TriphenylphosphineHCID 230765624-(Chloromethyl)-1-ethyl-1H-pyrazole hydrochloride

生成物 1

HCID 23076402HCID 23076402、化合物収率 95%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 4-chloromethyl-1-ethyl-1H-pyrazole hydrochloride (24.00 g), triphenylphosphine (34.10 g), acetonitrile (250 mL) was heated under reflux for 16 hrs. The reaction mixture was concentrated, and the residue was decanted and washed with diethyl ether (3 times with 200 mL). Toluene was added and the mixture was concentrated under reduced pressure to give [(1-ethyl-1H-pyrazol-4-yl)methyl](triphenyl)phosphonium chloride hydrochloride as amorphous form (57.47 g, yield 95%). NMR (DMSO-d6) δ: 1.22 (3H, t, J=7.2 Hz), 4.01 (2H, q, J=7.2 Hz), 4.66 (1H,brs), 5.01 (2H, d, J=13.8 Hz), 6.93 (1H, s), 7.25 (1H, s), 7.68-7.79 (12H, m), 7.87-7.92 (3H, m).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hrs
  3. concentrationThe reaction mixture was concentrated
  4. customthe residue was decanted
  5. washwashed with diethyl ether (3 times with 200 mL)
  6. additionToluene was added
  7. concentrationthe mixture was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-af0eaadfa5df46e89af94934f84349ca
出典データセット
uspto-grants-2008_05
特許番号
US07368578B2

反応ノート

読み込み中…