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Trifluoroacetic acid → HCID 21268184, 화합물

HRID 1779657
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HRID 1779657 반응식
[N+:1]([C:4]1[CH:12]=[C:11]2[C:7]([C:8]([C:13]3[CH2:14][CH2:15][NH:16][CH2:17][CH:18]=3)=[CH:9][NH:10]2)=[CH:6][CH:5]=1)([O-:3])=[O:2].C([SiH](CC)CC)C.[F:26][C:27]([F:32])([F:31])[C:28]([OH:30])=[O:29]>>[F:26][C:27]([F:32])([F:31])[C:28]([OH:30])=[O:29].[N+:1]([C:4]1[CH:12]=[C:11]2[C:7]([C:8]([CH:13]3[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]3)=[CH:9][NH:10]2)=[CH:6][CH:5]=1)([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 212682696-Nitro-3-(1,2,3,6-tetrahydro-4-pyridinyl)-1H-indole

생성물 1

HCID 21268184HCID 21268184, 화합물

실험 절차

6-nitro-3-(1,2,3,6-tetrahydropyridin-4-yl)-1H-indole (2.4 g, 9.9 mmol) was stirred in trifluoroacetic acid (10 mL) at room temperature under an atmosphere of nitrogen. Triethylsilane (1.65 mL, 10.4 mmol) was slowly added. After an initial exotherm, the mixture was stirred at room temperature for 12 hours. The mixture was concentrated under reduced pressure to yield a dark residue. The crude product was crystallized from ethanol to yield the title compound as a yellow crystalline solid. Yield 2.4 g (67%). mp 215°-217° C. FDMS m/e=245 (M+ of free base).

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customto yield a dark residue
  3. customThe crude product was crystallized from ethanol

출처 및 근거

ORD 기록
ord-5629b0520705424eaee99d439b9e00e6
출처 데이터셋
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05627196

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