Dimethylformamide → HCID 136340694, 화합물

HRID 570967노트

반응식

HRID 570967 반응식
N1CCCCC1.[CH3:7][C:8]1[N:9]=[CH:10][NH:11][C:12]=1[N+:13]([O-:15])=[O:14].[S:16]1[CH:20]=[CH:19][CH:18]=[C:17]1[CH:21]=O.CN(C=O)C>CC(O)C>[N+:13]([C:12]1[NH:11][CH:10]=[N:9][C:8]=1/[CH:7]=[CH:21]/[C:17]1[S:16][CH:20]=[CH:19][CH:18]=1)([O-:15])=[O:14]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 73642-ThiophenecarboxaldehydeHCID 8082PiperidineHCID 862781031H-Imidazole, 4-methyl-5-nitro-

생성물 1

HCID 136340694HCID 136340694, 화합물수율 69%

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
100 °C

실험 절차

Piperidine (1.7 g, 0.02 mol) was added to a suspension of 4-methyl-5-nitroimidazole (5 g, 0.04 mol) and 2-thiophenecarboxaldehyde (22 g, 0.2 mol) and heated at 100° C. for 15 hours. After cooling, DMF (5 mL) and IPA (15 mL) were added and the precipitate filtered from solution and washed with IPA (50 mL) to leave the product as a yellow solid (6.0 g, 69%). δH (DMSO-d6) 13.56 (1H, bs, NH), 7.90 (1H, s), 7.66 (1H, d, J=16.4), 7.66 (1H, d, J=5.0), 7.40 (1H, d, J=16.4), 7.35 (1H, d, J=3.6), 7.15 (1H, dd, J=3.6, 5.0).

후처리

  1. temperatureAfter cooling
  2. filtrationthe precipitate filtered from solution
  3. washwashed with IPA (50 mL)

출처 및 근거

ORD 기록
ord-e935b2b20cf84af9b2f6f47c60e553a9
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09024018B2

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