Methanol → HCID 19937767, 화합물

HRID 36763

반응식

HRID 36763 반응식
[CH:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH:10]([CH3:12])[CH3:11])[C:5]=1[NH:13][C:14](=[O:20])[CH2:15][S:16][C:17](=O)[CH3:18])([CH3:3])[CH3:2].CO.[OH-].[Na+].BrCC[CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][N:38]1[CH2:43][CH2:42][N:41]([C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)[CH2:40][CH2:39]1>C(OCC)(=O)C>[CH:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH:10]([CH3:12])[CH3:11])[C:5]=1[NH:13][C:14](=[O:20])[CH2:15][S:16][CH2:17][CH2:18][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][N:38]1[CH2:43][CH2:42][N:41]([C:44]2[CH:45]=[CH:46][CH:47]=[CH:48][CH:49]=2)[CH2:40][CH2:39]1)([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 887Methanol2회HCID 14798Sodium HydroxideHCID 15289526HCID 15289526, 화합물HCID 199377541-Bromo-12-(4-phenylpiperazinyl)dodecane

생성물 1

HCID 19937767HCID 19937767, 화합물수율 57.2%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of 1.47 g of N-(2,6-diisopropylphenyl)-2-(acetylthio)acetamide and 12 ml of methanol was added dropwise 1.7 ml of a 30% aqueous sodium hydroxide solution at 0° C. in an argon atmosphere. After stirring for 30 minutes, a mixture of 2.05 g of 1-bromo-12-(4-phenylpiperazinyl)dodecane synthesized in (1) above and 14 ml of methanol was added thereto, followed by stirring at 60° C. for 1 hour and then at room temperature for 16 hours. To the reaction mixture was added 100 ml of ethyl acetate, and the mixture was washed successively with water and a saturated sodium chloride aqueous solution, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was subjected to column chromatography using a 1:2 mixture of ethyl acetate and hexane as a developing solvent. The resulting crystals were recrystallized from isopropyl alcohol-water to yield 1.66 g of the title compound as white powder (m.p.=76.5° -77.5° C.).

후처리

  1. stirringby stirring at 60° C. for 1 hour
  2. waitat room temperature for 16 hours
  3. washthe mixture was washed successively with water
  4. dry with materiala saturated sodium chloride aqueous solution, and dried over magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. additiona 1:2 mixture of ethyl acetate and hexane as a developing solvent
  7. customThe resulting crystals were recrystallized from isopropyl alcohol-water

출처 및 근거

ORD 기록
ord-84b459ec96ee44ad9b0841d016b96fa3
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05416212

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