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

Triethylamine → HCID 69519963, 화합물

HRID 1179941
노트
인쇄 미리보기

반응식

HRID 1179941 반응식
[OH:1][C:2]1[N:7]=[CH:6][C:5]([N:8]2[C:13](=[O:14])[CH2:12][C:11]([CH3:16])([CH3:15])[CH2:10][C:9]2=[O:17])=[CH:4][CH:3]=1.C(NC1C=CC([O:33][C:34]([N:36]2[CH2:41][CH2:40][CH:39]([O:42][Si](C(C)(C)C)(C)C)[CH2:38][CH2:37]2)=O)=NC=1)(=O)C1C=CC=CC=1.C(N(CC)CC)C.C(OCC)(=O)C>CN(C)C=O.Cl>[CH3:16][C:11]1([CH3:15])[CH2:12][C:13](=[O:14])[N:8]([C:5]2[CH:6]=[N:7][C:2]([O:1][C:34]([N:36]3[CH2:41][CH2:40][CH:39]([OH:42])[CH2:38][CH2:37]3)=[O:33])=[CH:3][CH:4]=2)[C:9](=[O:17])[CH2:10]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 695176994-(tert-Butyl-dimethyl-silanyloxy)-piperidine-1-carboxylic Acid 5-benzoylamino-pyridin-2-yl EsterHCID 178426979HCID 178426979, 화합물

생성물 1

HCID 69519963HCID 69519963, 화합물수율 25.2%

시약·촉매·용매 2

HCID 313
Hydrochloric Acid
용매
HCID 6228Dimethylformamide용매

실험 절차

A solution of 6′-hydroxy-4,4-dimethyl-4,5-dihydro-3H-[1,3′]bipyridinyl-2,6-dione (468 mg, 2.00 mmol), 4-(tert-butyl-dimethyl-silanyloxy)-piperidine-1-carboxylic acid 5-benzoylamino-pyridin-2-yl ester (0.90 g, 2.00 mmol) and triethylamine (0.20 g, 2.00 mmol) in dimethylformamide (10 mL) was stirred at room temperature for 18 hours. The solvent was evaporated in vacuo. The residue was dissolved in ethyl acetate, filtered over a short pad of silicagel and washed with ethyl acetate. The solvent was evaporated in vacuo and the residue was dissolved in 1 N HCl in ethyl acetate (10 mL, 10.0 mmol). After stirring for 1.5 hours at room temperature the solvent was evaporated in vacuo. The white solid was washed with a small amount of ethyl acetate and diethyl ether and dissolved in a few milliliters of dichloromethane and triethylamine (1 mL). Purification by flash column chromatography (SiO2, ethyl acetate:acetone 90:10) yielded the title compound (182 mg, 25% yield) as a white solid.

후처리

  1. customThe solvent was evaporated in vacuo
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. filtrationfiltered over a short pad of silicagel
  4. washwashed with ethyl acetate
  5. customThe solvent was evaporated in vacuo
  6. customwas evaporated in vacuo
  7. washThe white solid was washed with a small amount of ethyl acetate and diethyl ether
  8. dissolutiondissolved in a few milliliters of dichloromethane
  9. customPurification by flash column chromatography (SiO2, ethyl acetate:acetone 90:10)

출처 및 근거

ORD 기록
ord-d46895e166a64cc3bbe95a592ddef92a
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07279470B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트