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

Sodium hydride → HCID 19369599, 화합물

HRID 849234
노트
인쇄 미리보기

반응식

HRID 849234 반응식
[C:1]([O:5][C:6]([NH:8][C:9]1[CH:14]=[C:13]([N:15]2[CH2:20][CH2:19][O:18][CH2:17][CH2:16]2)[CH:12]=[C:11]([CH2:21][CH2:22][C:23]2[S:24][C:25]([CH2:29][CH3:30])=[C:26]([CH3:28])[N:27]=2)[N:10]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].[Cl:33][C:34]1[CH:35]=[C:36]([CH:41]=[C:42]([CH2:44]Cl)[CH:43]=1)[C:37]([O:39][CH3:40])=[O:38]>CN(C)C=O.C(OCC)(=O)C>[C:1]([O:5][C:6]([N:8]([C:9]1[CH:14]=[C:13]([N:15]2[CH2:16][CH2:17][O:18][CH2:19][CH2:20]2)[CH:12]=[C:11]([CH2:21][CH2:22][C:23]2[S:24][C:25]([CH2:29][CH3:30])=[C:26]([CH3:28])[N:27]=2)[N:10]=1)[CH2:44][C:42]1[CH:41]=[C:36]([C:37]([O:39][CH3:40])=[O:38])[CH:35]=[C:34]([Cl:33])[CH:43]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 24758Sodium hydrideHCID 19369740HCID 19369740, 화합물HCID 19369759Methyl 3-chloro-5-(chloromethyl)benzoate

생성물 1

HCID 19369599HCID 19369599, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 8857Ethyl Acetate
용매

실험 절차

2-tert-butoxycarbonylamino-6-[2-(5-ethyl-4-methyl-1,3-thiazol-2-yl)ethyl]-4-morpholinopyridine (500 mg) obtained in Example 109-(1) was dissolved in dimethylformamide (12 ml), and 60% sodium hydride (58 mg) was added under cooling with ice, followed by stirring at room temperature for one hour. The reaction solution was cooled with ice, and a solution of methyl 3-chloro-5-chloromethylbenzoate (438 mg) in dimethylformamide (5 ml), was added thereto, followed by stirring at room temperature for 13 hours. The reaction solution was diluted with ethyl acetate, washed with water and a saturated sodium chloride aqueous solution and then, dried over anhydrous magnesium sulfate. Then, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/2) to obtain the above identified compound (628 mg).

후처리

  1. temperatureunder cooling with ice
  2. temperatureThe reaction solution was cooled with ice
  3. stirringby stirring at room temperature for 13 hours
  4. washwashed with water
  5. dry with materiala saturated sodium chloride aqueous solution and then, dried over anhydrous magnesium sulfate
  6. distillationThen, the solvent was distilled off under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/2)
  8. customto obtain the

출처 및 근거

ORD 기록
ord-fd60ffbfbadc4d0bbb92b158e250d523
출처 데이터셋
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06011039

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트