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Imidazole → HCID 59750865, 화합물

HRID 748797
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HRID 748797 반응식
[OH:1][CH2:2][CH2:3][N:4]([CH2:12][CH2:13][OH:14])[C:5](=[O:11])[O:6][C:7]([CH3:10])([CH3:9])[CH3:8].N1C=CN=C1.[C:20]([Si:24](Cl)([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)([CH3:23])([CH3:22])[CH3:21].CCCCCC>ClCCl.CN(C)C=O.C(OCC)(=O)C>[Si:24]([O:1][CH2:2][CH2:3][N:4]([CH2:12][CH2:13][OH:14])[C:5](=[O:11])[O:6][C:7]([CH3:8])([CH3:9])[CH3:10])([C:20]([CH3:23])([CH3:22])[CH3:21])([C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 795ImidazoleHCID 8058HexaneHCID 94078tert-ButyldiphenylchlorosilaneHCID 4360601N-Boc-diethanolamine

생성물 1

HCID 59750865HCID 59750865, 화합물수율 54%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매
HCID 22350042
dichloromethane N,N-dimethylformamide
용매

실험 절차

In a dichloromethane/N,N-dimethylformamide (70 ml/70 ml) mixture were dissolved t-butyl N,N-bis(2-hydroxyethyl)carbamate (9.00 g, 43.8 mmol) and imidazole (2.60 g, 38.2 mmol), followed by the dropwise addition of t-butylchlorodiphenylsilane (8.1 ml, 31 mmol) at room temperature. After completion of the dropwise addition, the reaction mixture was stirred at room temperature for 14 hours. The residue obtained by concentrating the reaction mixture under reduced pressure was added with diethyl ether. The resulting mixture was washed with water and the organic layer was dried over anhydrous magnesium sulfate. After filtration, the filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to flash silica gel chromatography, and the fraction obtained from the hexane:ethyl acetate=2:1 eluate was concentrated under reduced pressure, whereby the title compound (7.41 g, 16.7 mmol, 54%) was obtained as a colorless oil.

후처리

  1. additionAfter completion of the dropwise addition
  2. customThe residue obtained
  3. concentrationby concentrating the reaction mixture under reduced pressure
  4. additionwas added with diethyl ether
  5. washThe resulting mixture was washed with water
  6. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  7. filtrationAfter filtration
  8. concentrationthe filtrate was concentrated under reduced pressure
  9. customThe residue thus obtained

출처 및 근거

ORD 기록
ord-5c5ca53811f642fea10bfd8baf26d2df
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07399775B2

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