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Dicyclohexylcarbodiimide → HCID 13748635, 화합물

HRID 1904632
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HRID 1904632 반응식
[C:1]([O:5][C:6](=[O:14])[CH2:7][NH:8][CH:9]1[CH2:13][CH2:12][CH2:11][CH2:10]1)([CH3:4])([CH3:3])[CH3:2].C1(N=C=NC2CCCCC2)CCCCC1.[C:30]1([S:36][CH2:37][CH:38]([CH3:42])[C:39](O)=[O:40])[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1>C1COCC1>[C:1]([O:5][C:6](=[O:14])[CH2:7][N:8]([C:39](=[O:40])[CH:38]([CH3:42])[CH2:37][S:36][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[CH:9]1[CH2:10][CH2:11][CH2:12][CH2:13]1)([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 127593292-Methyl-3-(phenylsulfanyl)propanoic acidHCID 13298943Tert-butyl 2-(cyclopentylamino)acetate

생성물 1

HCID 13748635HCID 13748635, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a cold solution of 19.9 g (0.1M) of N-cyclopentyl glycine-t-butyl ester in 200 ml THF was added 26 g dicyclohexyl carbodiimide. After stirring for 1/2 hour, a solution of 19.6 g (0.1M) of 3-phenylthio-2-methyl propanoic acid in 50 ml THF was added and stirring continued for 16 hours. It was then filtered, solvent removed, dissolved in ether, washed well with water, filtered, dried over MgSO4, and evaporated to dryness leaving an oily residue which was purified by HPLC using ethyl acetate-hexane (3:17) as eluent.

후처리

  1. stirringstirring
  2. waitcontinued for 16 hours
  3. filtrationIt was then filtered
  4. customsolvent removed
  5. dissolutiondissolved in ether
  6. washwashed well with water
  7. filtrationfiltered
  8. dry with materialdried over MgSO4
  9. customevaporated to dryness
  10. customleaving an oily residue which
  11. customwas purified by HPLC

출처 및 근거

ORD 기록
ord-67cd49e6605e4bf596b9a6c3a92b3cef
출처 데이터셋
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04839367

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