Triethylamine → HCID 22272721, 화합물

HRID 1064855노트

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HRID 1064855 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 22272721HCID 22272721, 화합물수율 83%

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

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온도
80 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-1cbfebdc123b44759f37fc3563ab58c5
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06969711B2

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