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

18-Crown-6 → HCID 59369326, 화합물

HRID 1689791
노트
인쇄 미리보기

반응식

HRID 1689791 반응식
[CH2:1]([O:3][C:4](=[O:19])[C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH2:17][CH2:16][CH2:15][CH:14]([OH:18])[CH2:13][CH2:12]2)=[CH:7][CH:6]=1)[CH3:2].C1OCCOCCOCCOCCOCCOC1.[K].Br[CH2:40][C:41]1[C:42]([C:49]2[C:54]([Cl:55])=[CH:53][CH:52]=[CH:51][C:50]=2[Cl:56])=[N:43][O:44][C:45]=1[CH:46]1[CH2:48][CH2:47]1>C(O)(C)(C)C.O1CCCC1>[CH2:1]([O:3][C:4](=[O:19])[C:5]1[CH:6]=[CH:7][C:8]([N:11]2[CH2:17][CH2:16][CH2:15][CH:14]([O:18][CH2:40][C:41]3[C:42]([C:49]4[C:50]([Cl:56])=[CH:51][CH:52]=[CH:53][C:54]=4[Cl:55])=[N:43][O:44][C:45]=3[CH:46]3[CH2:48][CH2:47]3)[CH2:13][CH2:12]2)=[CH:9][CH:10]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 2855718-Crown-6HCID 5462222PotassiumHCID 593693284-(Bromomethyl)-5-cyclopropyl-3-(2,6-dichlorophenyl)isoxazoleHCID 669062524-(4-Hydroxy-azepan-1-yl)-benzoic acid ethyl ester

생성물 1

HCID 59369326HCID 59369326, 화합물

시약·촉매·용매 2

HCID 6386
tert-Butanol
용매
HCID 8028Tetrahydrofuran용매

실험 절차

Anhydrous tetrahydrofuran (5 mL) is added at room temperature to a mixture of 4-(4-hydroxy-azepan-1-yl)-benzoic acid ethyl ester (364 mg, 1.38 mmol), 18-crown-6 (407 mg, 1.52 mmol) and tert-butyl alcohol, potassium derivative (178 mg, 1.52 mmol). The mixture is stirred for 5 minutes and then 4-bromomethyl-5-cyclopropyl-3-(2,6-dichloro-phenyl)-isoxazole (480 mg, 1.38 mmol) is added. After 1.5 h, the solvent is removed and water is added. The aqueous phase is extracted with ethyl acetate. The organic layers are combined, dried over anhydrous sodium sulfate, filtered, and the solvent is removed under reduced pressure. The residue is purified via flash chromatography (40 g silica) eluting with a gradient of ethyl acetate/hexane (0% to 30%) to provide the title compound as a colorless waxy solid (203 mg, 28%). ES/MS m/z 529.0 (M+1).

후처리

  1. waitAfter 1.5 h
  2. customthe solvent is removed
  3. additionwater is added
  4. extractionThe aqueous phase is extracted with ethyl acetate
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customthe solvent is removed under reduced pressure
  8. customThe residue is purified via flash chromatography (40 g silica)
  9. washeluting with a gradient of ethyl acetate/hexane (0% to 30%)

출처 및 근거

ORD 기록
ord-c7eab4bc2f9d4f3aa4c0919cb2ffbe4e
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08153624B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트