Triethylamine → HCID 22272721、化合物

HRID 1064855ノート

反応式

HRID 1064855 の反応式
[CH3:1][S:2][C:3]1[C:8]([NH:9][C:10](=[O:18])OC2C=CC=CC=2)=[C:7]([S:19][CH3:20])[CH:6]=[C:5]([CH3:21])[N:4]=1.C(N(CC)CC)C.[CH2:29]([NH:36][CH2:37][CH2:38][N:39]1[CH2:44][CH2:43][N:42]([CH2:45][CH2:46][CH2:47][OH:48])[CH2:41][CH2:40]1)[CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35]>C1(C)C=CC=CC=1.O>[CH3:1][S:2][C:3]1[C:8]([NH:9][C:10](=[O:18])[N:36]([CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])[CH2:37][CH2:38][N:39]2[CH2:44][CH2:43][N:42]([CH2:45][CH2:46][CH2:47][OH:48])[CH2:41][CH2:40]2)=[C:7]([S:19][CH3:20])[CH:6]=[C:5]([CH3:21])[N:4]=1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 22272787HCID 22272787、化合物HCID 54132991Phenyl [6-methyl-2,4-bis(methylsulfanyl)pyridin-3-yl]carbamate

生成物 1

HCID 22272721HCID 22272721、化合物収率 83%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

To a solution of this phenyl carbamate (188 mg, 0.59 mmol) in toluene (3 ml) were added triethylamine (72 mg, 0.71 mmol) and 3-[4-(2-heptylaminoethyl)piperazin-1-yl]propanol (168 mg, 0.59 mmol) and the mixture was stirred at 80° C. for 3 hours. The reaction solution was diluted with water and extracted with chloroform. The organic layer was washed with water and a saturated sodium chloride solution successively, dried over anhydrous sodium sulfate and concentrated in vacuo. The resulting residue was purified by a silica gel column chromatography (silica gel 15 g, developing solvent; chloroform:methanol=40:1 10:1) to provide 249 mg (yield 83%) of N′-[2,4-bis(methylthio)-6-methyl-3-pyridyl]-N-heptyl-N-[2-[4-(3-hydroxypropyl)piperazin-1-yl]ethyl]urea as colorless oil.

後処理

  1. extractionextracted with chloroform
  2. washThe organic layer was washed with water
  3. dry with materiala saturated sodium chloride solution successively, dried over anhydrous sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe resulting residue was purified by a silica gel column chromatography (silica gel 15 g, developing solvent; chloroform:methanol=40:1 10:1)

出典と根拠

ORDレコード
ord-1cbfebdc123b44759f37fc3563ab58c5
出典データセット
uspto-grants-2005_11
特許番号
US06969711B2

反応ノート

読み込み中…