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Triethylamine → Tert-butyl n-[(phenylcarbamoyl)methyl]carbamate

HRID 1700350
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HRID 1700350 반응식
Cl.CN(C)CCCN=C=NCC.O[N:14]1[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2N=N1.C(N(CC)CC)C.[C:30]([O:34][C:35]([NH:37][CH2:38][C:39](O)=[O:40])=[O:36])([CH3:33])([CH3:32])[CH3:31]>ClCCl.C(OCC)(=O)C>[C:18]1([NH:14][C:39]([CH2:38][NH:37][C:35](=[O:36])[O:34][C:30]([CH3:32])([CH3:31])[CH3:33])=[O:40])[CH:17]=[CH:22][CH:21]=[CH:20][CH:19]=1
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참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 78288N-(tert-butoxycarbonyl)glycineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

생성물 1

HCID 10634424Tert-butyl n-[(phenylcarbamoyl)methyl]carbamate

시약·촉매·용매 2

HCID 6344
Dichloromethane
용매
HCID 8857Ethyl Acetate용매

실험 절차

1.27 g (1.19 mmol) of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, 681 mg (5.04 mmol) of 1-hydroxybenzotriazole and 0.95 ml (6.82 mmol) of triethylamine were added to 1.15 g (6.56 mmol) of t-butoxycarbonylglycine in 20 ml of dichloromethane under cooling in an ice bath, and they were stirred at room temperature overnight. Ethyl acetate was added to the reaction mixture, and the product was washed with 0.1 N hydrochloric acid and then with a saturated aqueous sodium hydrogencarbonate solution. The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure to obtain the title compound.

후처리

  1. temperatureunder cooling in an ice bath
  2. washthe product was washed with 0.1 N hydrochloric acid
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-94afdbd7c5104b669ac7bff43f1510da
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06350762B1

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