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

2,4,6-Trimethylaniline → HCID 11452287, 화합물

HRID 2216301
노트
인쇄 미리보기

반응식

HRID 2216301 반응식
[CH3:1][C:2]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH3:10])[C:3]=1[NH2:4].C[Si]([N-][Si](C)(C)C)(C)C.[Na+].Cl[C:22]1[C:27]([S:28]([C:31]2[CH:36]=[CH:35][C:34]([O:37][CH3:38])=[CH:33][CH:32]=2)(=[O:30])=[O:29])=[CH:26][N:25]=[C:24]([CH3:39])[N:23]=1>C1COCC1>[CH3:38][O:37][C:34]1[CH:33]=[CH:32][C:31]([S:28]([C:27]2[C:26]([NH:4][C:3]3[C:5]([CH3:10])=[CH:6][C:7]([CH3:9])=[CH:8][C:2]=3[CH3:1])=[N:25][C:24]([CH3:39])=[N:23][CH:22]=2)(=[O:29])=[O:30])=[CH:36][CH:35]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 69132,4,6-TrimethylanilineHCID 2724254Sodium bis(trimethylsilyl)amideHCID 21941670HCID 21941670, 화합물

생성물 1

HCID 11452287HCID 11452287, 화합물수율 45.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

To a solution of 2,4,6-trimethylaniline (0.089 mL, 0.64 mmol) in THF (2 mL), NaHMDS (1.0 M in THF, 0.64 mL, 0.64 mmol) was added dropwise at 0° C. The mixture was stirred under N2 at 0° C. for 10 min, and then 4-chloro-5-(4-methoxy-benzenesulfonyl)-2-methyl-pyrimidine (158 mg, 0.53 mmol) in THF (3 mL) was added dropwise at 0° C. The reaction mixture was stirred at room temperature for 1 h, and then quenched with saturated ammonium chloride. The organic layer was separated and the aqueous layer was extracted with ethyl acetate (2×). The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by chromatography on silica gel (1:2 ethyl acetate/hexanes) to provide the target compound (95 mg, 45%) as a light yellow solid: mp 153–155° C.; 1H NMR (300 MHz, CDCl3) δ 8.74 (s 1H), 8.22 (br s, 1H), 7.88 (d, J=7.0 Hz, 2H), 6.98 (d, J=7.0 Hz, 1H), 6.91 (s, 2H), 3.86 (s, 3H), 2.38 (s, 3H), 2.30 (s, 3H), 2.01 (s, 6H); ESI MS m/z 398 [(M+H)+, calcd for C21H24N3O3S, 398.2].

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 1 h
  2. customquenched with saturated ammonium chloride
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted with ethyl acetate (2×)
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by chromatography on silica gel (1:2 ethyl acetate/hexanes)

출처 및 근거

ORD 기록
ord-955bd7e86fd44bfdb0062bd459a4a00b
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07112585B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트