Methanol → HCID 19937767、化合物

HRID 36763

反応式

HRID 36763 の反応式
[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]

参加物

6

反応物 4

HCID 887Methanol2 回HCID 14798Sodium HydroxideHCID 15289526HCID 15289526、化合物HCID 199377541-Bromo-12-(4-phenylpiperazinyl)dodecane

生成物 1

HCID 19937767HCID 19937767、化合物収率 57.2%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-84b459ec96ee44ad9b0841d016b96fa3
出典データセット
uspto-grants-1995_05
特許番号
US05416212

関連ノート

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