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Triphenylphosphine → HCID 19802562, 화합물

HRID 1645817
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HRID 1645817 반응식
O[CH:2]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH2:3][N:4]1[CH2:9][CH2:8][N:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[O:16][CH3:17])[CH2:6][CH2:5]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[NH:43]1[CH2:47][CH2:46][CH2:45][CH2:44]1.CCOC(/N=N/C(OCC)=O)=O>ClCCl>[CH3:17][O:16][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[N:7]1[CH2:8][CH2:9][N:4]([CH2:3][CH:2]([N:43]2[CH2:47][CH2:46][CH2:45][CH2:44]2)[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH2:5][CH2:6]1
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참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 31268PyrrolidineHCID 5462977Diethyl azodicarboxylateHCID 163323132-[4-(2-methoxyphenyl)piperazin-1-yl]-1-phenylethanol

생성물 1

HCID 19802562HCID 19802562, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0.5 °C

실험 절차

A mixture of 1-(2-hydroxy-2-phenylethyl)-4-(2-methoxyphenyl)-piperazine (5.65 g; 0.018 m), triphenylphosphine (5.69 g, 0.022m) and pyrollidine (15 ml; 0.18 m) in dichloromethane (100 ml) was stirred at 0.5° C. and a solution of diethylazodicarboxylate (3.8 ml, 0.024 m) in dichloromethane (5 ml) was added over 5 minutes. The resulting yellow solution was stirred at ambient temperature for 48 hrs. The residue on evaporation was partitioned between ether and 3N aq. hydrochloric acid. The combined HCl layers were washed with ether and then basified with ammonia and shaken with 3 portions of ether. The ether layers were washed well with water and dried over magnesium sulfate to give an oil which was chromatographed to give 0.96 g of the title compound. The crude oil in ethanol was acidified with ethanolic hydrogen chloride. The solvent was evaporated, and the residual foam solidified when triturated with ethanol and ether. The solid was recrystallised from ethanol to give the title compound as the dihydrochloride (0.45 g), m.p. 214°-18° C(d).

후처리

  1. stirringThe resulting yellow solution was stirred at ambient temperature for 48 hrs
  2. customThe residue on evaporation
  3. customwas partitioned between ether and 3N aq. hydrochloric acid
  4. washThe combined HCl layers were washed with ether
  5. stirringshaken with 3 portions of ether
  6. washThe ether layers were washed well with water
  7. dry with materialdried over magnesium sulfate
  8. customto give an oil which
  9. customwas chromatographed

출처 및 근거

ORD 기록
ord-e467bae9c7c7407b90d2a6935574e9cb
출처 데이터셋
uspto-grants-1993_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05177078

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