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Triethylamine → 4-[Ethyl-(2-methanesulfonyloxy-ethyl)-amino]-6-methyl-2-(2,4,6-trimethyl-phenoxy)-nicotinic acid methyl ester

HRID 967990
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인쇄 미리보기

반응식

HRID 967990 반응식
[CH3:1][O:2][C:3](=[O:27])[C:4]1[C:9]([N:10]([CH2:14][CH3:15])[CH2:11][CH2:12][OH:13])=[CH:8][C:7]([CH3:16])=[N:6][C:5]=1[O:17][C:18]1[C:23]([CH3:24])=[CH:22][C:21]([CH3:25])=[CH:20][C:19]=1[CH3:26].[CH3:28][S:29](Cl)(=[O:31])=[O:30].C(N(CC)CC)C>C(Cl)Cl>[CH3:1][O:2][C:3](=[O:27])[C:4]1[C:9]([N:10]([CH2:14][CH3:15])[CH2:11][CH2:12][O:13][S:29]([CH3:28])(=[O:31])=[O:30])=[CH:8][C:7]([CH3:16])=[N:6][C:5]=1[O:17][C:18]1[C:23]([CH3:24])=[CH:22][C:21]([CH3:25])=[CH:20][C:19]=1[CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 695875454-[Ethyl-(2-hydroxy-ethyl)-amino]-6-methyl-2-(2,4,6-trimethyl-phenoxy)-nicotinic acid methyl ester

생성물 1

HCID 865964814-[Ethyl-(2-methanesulfonyloxy-ethyl)-amino]-6-methyl-2-(2,4,6-trimethyl-phenoxy)-nicotinic acid methyl ester

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

실험 절차

A mixture of 4-[ethyl-(2-hydroxy-ethyl)-amino]-6-methyl-2-(2,4,6-trimethyl-phenoxy)-nicotinic acid methyl ester, methanesulfonyl chloride and triethylamine in methylene chloride was stirred at rt until all starting material was consumed. The mixture was quenched with water, brine and extracted with methylene chloride. The organic layer was dried and concentrated to dryness. The residue was purified through silica gel column chromatography to give the title compound. 1H NMR(CDCl3) d 6.83(s, 2H), 6.25(s, 1H), 4.34(t, 2H), 3.86(s, 3H), 3.6(t, 2H), 3.38(t, 2H), 3.09s, 3H), 2.25(s, 3H), 2.20(s, 3H), 2.04(s, 6H), 1.18(t, 3H) ppm.

후처리

  1. customwas consumed
  2. customThe mixture was quenched with water, brine
  3. extractionextracted with methylene chloride
  4. customThe organic layer was dried
  5. concentrationconcentrated to dryness
  6. customThe residue was purified through silica gel column chromatography

출처 및 근거

ORD 기록
ord-d6f3806b51664efa859b5d15185d6665
출처 데이터셋
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06956047B1

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