홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Dimethylamine → ((1S)-5-acetylamino-1-(dimethylcarbamoyl)pentyl)carbamic acid tert-butyl ester

HRID 365431
노트
인쇄 미리보기

반응식

HRID 365431 반응식
[C:1]([NH:4][CH2:5][CH2:6][CH2:7][CH2:8][C@H:9]([NH:13][C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[C:10]([OH:12])=O)(=[O:3])[CH3:2].O.ON1C2C=CC=CC=2N=N1.Cl.[CH3:33][N:34](C)[CH2:35]CCN=C=NCC.CNC.CO>ClCCl.CN(C)C=O.C(OCC)(=O)C>[C:17]([O:16][C:14](=[O:15])[NH:13][C@H:9]([C:10](=[O:12])[N:34]([CH3:35])[CH3:33])[CH2:8][CH2:7][CH2:6][CH2:5][NH:4][C:1](=[O:3])[CH3:2])([CH3:20])([CH3:19])[CH3:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 674DimethylamineHCID 887MethanolHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 7016049Boc-Lys(Ac)-OH

생성물 1

HCID 53944459((1S)-5-acetylamino-1-(dimethylcarbamoyl)pentyl)carbamic acid tert-butyl ester
수율 55%

시약·촉매·용매 3

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

반응 조건

온도
0 °C

실험 절차

(2S)-6-Acetylamino-2-(tert-butoxycarbonylamino)hexanoic acid (Purchased at Bachem, 5.0 g, 17.3 mmol) was dissolved in dichloromethane (100 ml) and N,N-dimethylformamide (50 ml). 1-Hydroxybenzotriazole hydrate (2.65 g, 17.3 mmol) was added. The solution was cooled to 0° C. N-(3-Dimethylaminopropyl)-N'-ethylcarbodiimide hydrochloride (3.32 g, 17.3 mmol) was added. The reaction mixture was stirred for 20 min at 0° C. A 33% solution or dimethylamine in methanol (16.4 ml, 121 mmol) was added. The reaction mixture was stirred for 16 h, while it was warming up to room temperature. It was diluted with ethyl acetate (250 ml) and washed with a 10% aqueous solution of sodium hydrogensulfate (200 ml). The aqueous phase was extracted with ethyl acetate (2×100 ml). The combined organic layers were washed with a saturated aqueous solution of sodium hydrogen carbonate (200 ml) and dried over magnesium sulfate. The solvent was removed. The crude product was purified by flash chromatography on silica (120 g), using dichloromethane/methanol (10:1) as eluent to give 3.00 g of ((1S)-5-acetylamino-1-(dimethylcarbamoyl)pentyl)carbamic acid tert-butyl ester.

후처리

  1. stirringThe reaction mixture was stirred for 16 h, while it
  2. temperaturewas warming up to room temperature
  3. washwashed with a 10% aqueous solution of sodium hydrogensulfate (200 ml)
  4. extractionThe aqueous phase was extracted with ethyl acetate (2×100 ml)
  5. washThe combined organic layers were washed with a saturated aqueous solution of sodium hydrogen carbonate (200 ml)
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent was removed
  8. customThe crude product was purified by flash chromatography on silica (120 g)

출처 및 근거

ORD 기록
ord-7acd336a14854691ae744e26b7aba77b
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06127341

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트