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Triethylamine → HCID 67582173, 화합물

HRID 580884
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HRID 580884 반응식
[C:1]([NH:8][CH2:9][C:10]([OH:12])=O)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].C(N(CC)CC)C.C(Cl)(=O)C(Cl)=O.[Cl:26][C:27]1[CH:28]=[C:29]([NH:33][CH2:34][C:35]([O:37][CH3:38])=[O:36])[CH:30]=[CH:31][CH:32]=1>ClCCl.CCOC(C)=O>[C:4]([O:3][C:1]([NH:8][CH2:9][C:10]([N:33]([C:29]1[CH:30]=[CH:31][CH:32]=[C:27]([Cl:26])[CH:28]=1)[CH2:34][C:35]([O:37][CH3:38])=[O:36])=[O:12])=[O:2])([CH3:5])([CH3:6])[CH3:7]
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참가 물질

7

반응물 4

HCID 8471Triethylamine2회HCID 65578Oxalyl chlorideHCID 78288N-(tert-butoxycarbonyl)glycineHCID 11629788HCID 11629788, 화합물

생성물 1

HCID 67582173HCID 67582173, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회
HCID 8857
Ethyl Acetate
용매

실험 절차

To a solution of Boc-glycine and triethylamine (1.0 equiv.) in dichloromethane at 0° C. is added oxalylchloride (1.0 equiv). After one hour, a solution of the product from Step F (1 equiv.) in dichloromethane is added to the first solution, followed by triethylamine (1 equiv.). The solution is allowed to warm to room temperature. After complete reaction, the solution is poured into EtOAc and washed with sat. NH4Cl soln., sat. NaHCO3 soln., and brine. The solution is dried (Na2SO4), filtered, and concentrated in vacuo. The resulting material is purified by silica gel chromatography to provide the titled compound.

후처리

  1. customAfter complete reaction
  2. washwashed with sat. NH4Cl soln
  3. dry with materialThe solution is dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe resulting material is purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-8dadbb4b93c4497397c169d9ffcda812
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05919785

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