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

Methyl iodide → HCID 66762091, 화합물

HRID 561781
노트
인쇄 미리보기

반응식

HRID 561781 반응식
[H-].[Na+].[Cl:3][C:4]1[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][OH:19])=[CH:13][C:5]=1[C:6]([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7].I[CH3:21]>C1COCC1>[Cl:3][C:4]1[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][O:19][CH3:21])=[CH:13][C:5]=1[C:6]([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 66761548HCID 66761548, 화합물

생성물 1

HCID 66762091HCID 66762091, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a suspension of sodium hydride (60% w/w dispersion in oil, 2 eq.) in anhydrous THF (0.23 M) was added tert-butyl 2-chloro-5-(2-hydroxyethyl)benzoate from the previous step (1 eq.). The reaction mixture was heated at reflux for 30 min before iodomethane (7.9 eq.) was added. After carefully quenching with sat. aq. NaHCO3, the resulting mixture was extracted with ether. The combined organic extracts were washed with brine, dried over MgSO4 and filtered. Concentration of the filtrate in vacuo afforded a cloudy oil. Purification of the crude product thus obtained by way of flash chromatography (SiO2, Hex→85:15 (v/v) Hex:EtOAc) afforded the title compound as a colorless oil.

후처리

  1. temperatureThe reaction mixture was heated
  2. additionwas added
  3. customAfter carefully quenching with sat. aq. NaHCO3
  4. extractionthe resulting mixture was extracted with ether
  5. washThe combined organic extracts were washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customConcentration of the filtrate in vacuo afforded a cloudy oil
  9. customPurification of the crude product
  10. customthus obtained by way of flash chromatography (SiO2, Hex→85:15 (v/v) Hex:EtOAc)

출처 및 근거

ORD 기록
ord-25ba587f4633400eae5dbee9a156fb76
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08063105B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트