Lawesson's reagent → HCID 88190249, 화합물

HRID 2306263노트

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HRID 2306263 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][C@H:10]([NH:13][C:14](=O)[CH2:15][C:16]2[N:17]=[CH:18][N:19]([C:21]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)([C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH:20]=2)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:50])=CC=1>C1(C)C=CC=CC=1>[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][C@H:10]([NH:13][C:14](=[S:50])[CH2:15][C:16]2[N:17]=[CH:18][N:19]([C:21]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)([C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH:20]=2)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 70171956HCID 70171956, 화합물

생성물 1

HCID 88190249HCID 88190249, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
50 °C

실험 절차

(S)-N-[1-(tert-Butoxycarbonyl)pyrrolidin-3-yl]-2-[1-(triphenylmethyl)-1H-imidazol-4-yl]acetamide, as described above in Step C, (1.27 g, 2.37 mmol) was dissolved in toluene (20 mL), Lawesson's Reagent (478 mg, 1.18 mmol) was added and the reaction mixture was heated to 50° C. for 5 hours. The mixture was concentrated in vacuo and the residue was chromatographed on silica gel, eluting with a gradient of CH2Cl2—1% to 5% MeOH—0.1% to 0.5% NH4OH, to yield the above-titled compound.

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue was chromatographed on silica gel
  3. washeluting with a gradient of CH2Cl2—1% to 5% MeOH—0.1% to 0.5% NH4OH

출처 및 근거

ORD 기록
ord-33654c74084943b6830b4d605237ec98
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06441017B1

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