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Diisopropylethylamine → HCID 136411679, 화합물

HRID 983806
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HRID 983806 반응식
[Br:1][C:2]1[C:3]([OH:22])=[C:4]([C:9](=O)[CH2:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=2)[CH:5]=[C:6]([CH3:8])[CH:7]=1.C(N(C(C)C)CC)(C)C.[NH:32]([C:34]1[CH:42]=[CH:41][C:37]([C:38]([NH2:40])=[NH:39])=[CH:36][CH:35]=1)[NH2:33]>CCO>[Br:1][C:2]1[C:3]([OH:22])=[C:4]([C:9](=[N:33][NH:32][C:34]2[CH:35]=[CH:36][C:37]([C:38]([NH2:40])=[NH:39])=[CH:41][CH:42]=2)[CH2:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=2)[CH:5]=[C:6]([CH3:8])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 22556975HCID 22556975, 화합물HCID 225569864-Hydrazino-benzamidine

생성물 1

HCID 136411679HCID 136411679, 화합물수율 90%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

For example, a solution of 1-(3-bromo-2-hydroxy-5-methyl-phenyl)-3-(4-nitro-phenyl)-propan-1-one 201 (1.48 g, 0.004 mol), EtOH (30 mL), diisopropylethylamine (Hunigs base)(3 mL), and 4-Hydrazino-benzamidine 200 (0.93 g, 0.004 mol) is heated at reflux for 4 hr. (reaction times can vary between 2 h to 18 h). The solution is cooled to ambient temperature, filtered, washed with 6N HCl (2×25 mL), and dried for 12-18 h in a vacuum oven to give a 90% yield of 4-{N′-[1-(3-bromo-2-hydroxy-5-methyl-phenyl)-3-(4-nitro-phenyl)-propylidene]-hydrazino}-benzamidine 202 as an off-white solid (1.78 g, 0.0036 mol).

후처리

  1. temperatureat reflux for 4 hr
  2. custom(reaction times can vary between 2 h to 18 h)
  3. filtrationfiltered
  4. washwashed with 6N HCl (2×25 mL)
  5. customdried for 12-18 h in a vacuum oven

출처 및 근거

ORD 기록
ord-f53fcb9b3edb4332b2c8abe7feaa84c6
출처 데이터셋
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06867200B1

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