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Hydrochloric Acid → HCID 178526907, 화합물

HRID 1756398
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인쇄 미리보기

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HRID 1756398 반응식
[C:1]([C:3]1[CH:22]=[CH:21][C:6]([CH2:7][C:8]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([N+:17]([O-:19])=[O:18])[CH:15]=3)[N:10]([CH3:20])[CH:9]=2)=[C:5]([O:23][CH3:24])[CH:4]=1)#[N:2].[N-:25]=[N+:26]=[N-:27].[Na+].Cl.C([N:32]([CH2:35]C)CC)C.Cl>CN1CCCC1=O>[CH3:24][O:23][C:5]1[CH:4]=[C:3]([C:1]2[NH:27][N:26]=[N:25][N:2]=2)[CH:22]=[CH:21][C:6]=1[CH2:7][C:8]1[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([N+:17]([O-:19])=[O:18])[CH:15]=2)[N:10]([CH3:20])[CH:9]=1.[N+:17]([C:35]1[NH:32][N:27]=[N:26][N:25]=1)([O-:19])=[O:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 11130Triethylamine hydrochlorideHCID 33557Sodium AzideHCID 233658773-(4-Cyano-2-methoxybenzyl)1-methyl-5-nitroindole

생성물 2

HCID 178488254HCID 178488254, 화합물HCID 178526907HCID 178526907, 화합물수율 590.3%

시약·촉매·용매

1
HCID 13387N-methyl-2-pyrrolidone용매

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온도
150 °C

실험 절차

A mixture of 3-(4-cyano-2-methoxybenzyl)-1-methyl-5-nitroindole (0.458 g.), sodium azide (0.741 g.), and triethylamine hydrochloride (0.785 g.) in dry N-methyl-2-pyrrolidinone (6 ml.), under nitrogen, was stirred and heated at 150° C. for 1.5 hours. The mixture was cooled to ambient temperature, 1N hydrochloric acid (25 ml.) added cautiously, while stirring, the precipitated solid isolated by filtration, washed with water and dried in vacuo to give 3-[2-methoxy-4-(1-H-tetrazol-5-yl)benzyl]-1-methyl-5nitroindole, (V) (0.484 g., 94%) as a yellow powder, m.p. 249°-250° C.; partial NMR (250 MHz, DMSO-d6): 3.82 (s,3H, NMe); 3.97(s,3H, OMe); 4.13(s,2H, ArCH2).

후처리

  1. temperatureThe mixture was cooled to ambient temperature
  2. stirringwhile stirring
  3. customthe precipitated solid isolated by filtration
  4. washwashed with water
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-0d815a2a097547a4aab2fb3fcd95c228
출처 데이터셋
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05440035

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