Triphenylphosphine → HCID 23076402, 화합물

HRID 2221662노트

반응식

HRID 2221662 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 23076402HCID 23076402, 화합물수율 95%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-af0eaadfa5df46e89af94934f84349ca
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07368578B2

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