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

3-Hydroxypyridine → [4-(3-Pyridyloxymethyl)-2-phenylbenzoyl]methionine methyl ester

HRID 2121204
노트
인쇄 미리보기

반응식

HRID 2121204 반응식
[H-].[Na+].[OH:3][C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1.[CH3:10][O:11][C:12](=[O:35])[C@H:13]([CH2:31][CH2:32][S:33][CH3:34])[NH:14][C:15](=[O:30])[C:16]1[CH:21]=[CH:20][C:19]([CH2:22]Br)=[CH:18][C:17]=1[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[OH-].[Na+]>CN(C=O)C>[CH3:10][O:11][C:12](=[O:35])[C@H:13]([CH2:31][CH2:32][S:33][CH3:34])[NH:14][C:15](=[O:30])[C:16]1[CH:21]=[CH:20][C:19]([CH2:22][O:3][C:4]2[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=2)=[CH:18][C:17]=1[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 79713-HydroxypyridineHCID 14798Sodium HydroxideHCID 24758Sodium hydrideHCID 54323738(4-Bromomethyl-2-phenylbenzoyl)methionine methyl ester

생성물 1

HCID 53962378[4-(3-Pyridyloxymethyl)-2-phenylbenzoyl]methionine methyl ester수율 25.7%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매
3회

실험 절차

To a 0° C. suspension in DMF (2 mL) of sodium hydride (90% in mineral oil, 38 mg, 0.95 mmol) was added a solution of 3-hydroxypyridine (95 mg, 1.0 mmol) in DMF (2 mL) dropwise and the mixture was stirred for 0.5 hours. A solution of (4-bromomethyl-2-phenylbenzoyl)methionine methyl ester (218 mg, 0.5 mmol) in DMF (1 mL) was added and the reaction mixture was stirred for 18 hours. The reaction mixture was poured into aqueous 2N sodium hydroxide and the mixture was extracted with ethyl acetate (3×). The combined organic extracts were dried, filtered and concentrated in vacuo. Chromatography on silica gel (60% ethyl acetate-hexanes, then ethyl acetate) gave [4-(3-pyridyloxymethyl)-2-phenylbenzoyl]methionine methyl ester (58 mg). 1H NMR (300 MHz, DMSO-d6) δ 12.66 (bs, 1H), 8.58 (d, 1H), 8.38 (d, 1H), 8.17 (dd, 1H), 7.30-7.56 (m, 10H), 5.29 (s, 2H), 4.29 (ddd, 1H), 2.23 (m, 2H), 1.98 (s, 3H), 1.84 (m, 2H). MS (CI NH3) m/e 454 (M+NH4)+, 437 (M+H)+. Anal calcd for C24H24N2O4S (+0.41 H2O): C, 64.94; H, 5.64; N, 6.31. Found: C, 64.94; H, 5.35; N,S 6.14.

후처리

  1. stirringthe reaction mixture was stirred for 18 hours
  2. extractionthe mixture was extracted with ethyl acetate (3×)
  3. customThe combined organic extracts were dried
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-29d4c57c898e47e7b82cf1869e29d5cd
출처 데이터셋
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06693123B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트