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

Bromine → 5-Methyl-2-[3-[2,6-dimethyl-4-(2-methyl-tetrazol-5-yl)phenoxy]-propyl]-2,5-dimethoxy-2,5-dihydrofuran

HRID 865694
노트
인쇄 미리보기

반응식

HRID 865694 반응식
C(=O)([O-])[O-].[Na+].[CH3:6][C:7]1([O:32][CH3:33])[O:11][C:10]([CH2:14][CH2:15][CH2:16][O:17][C:18]2[C:23]([CH3:24])=[CH:22][C:21]([C:25]3[N:26]=[N:27][N:28]([CH3:30])[N:29]=3)=[CH:20][C:19]=2[CH3:31])([O:12][CH3:13])[CH:9]=[CH:8]1.[Na+].CC1OC(CCCOC2C(C)=CC(C3N=NN(C)N=3)=CC=2C)=CC=1.BrBr>CO.[Cl-].[Na+].O>[CH3:6][C:7]1([O:32][CH3:33])[O:11][C:10]([CH2:14][CH2:15][CH2:16][O:17][C:18]2[C:23]([CH3:24])=[CH:22][C:21]([C:25]3[N:26]=[N:27][N:28]([CH3:30])[N:29]=3)=[CH:20][C:19]=2[CH3:31])([O:12][CH3:13])[CH:9]=[CH:8]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 24408BromineHCID 52730885-[3,5-Dimethyl-4-[3-(5-methyl-2-furyl)propoxy]phenyl]-2-methyl-tetrazoleHCID 677670605-Methyl-2-[3-[2,6-dimethyl-4-(2-methyl-tetrazol-5-yl)-phenoxy]-propyl]-2,5 dimethoxy-2,5-dihydrofuran Sodium carbonate

생성물 1

HCID 229153545-Methyl-2-[3-[2,6-dimethyl-4-(2-methyl-tetrazol-5-yl)phenoxy]-propyl]-2,5-dimethoxy-2,5-dihydrofuran수율 87%

시약·촉매·용매 2

HCID 887Methanol용매2회
HCID 57417360Sodium chloride; water용매

실험 절차

5-Methyl-2-[3-[2,6-dimethyl-4-(2-methyl-tetrazol-5-yl)-phenoxy]-propyl]-2,5 dimethoxy-2,5-dihydrofuran Sodium carbonate (1.2 g) was added to a cooled (-10° C.) solution of 5-methyl 2-[3-[2,6-dimethyl-4-(2-methyl-tetrazol-5-yl)-phenoxy]-propyl]furan from example 9d (780 mg, 2.4 mmol) in 18 mL of methanol with stirring, and then bromine (0.135 g, 14 mmol) in 8 mL of methanol was added dropwise until the brown color persisted, and the resulting reaction mixture was allowed to stir at -10° C. for 45 min. To the mixture was added brine, extracted with ether (3×25 mL), and the organic layer was washed with water, dried over magnesium sulfate, and concentrated in vacuo to yield an oil which was purified by MPLC chromatography (ethyl acetate/hexane 3:7) to afford 820 mg (76.3%) of 5-methyl-2-[3-[2,6-dimethyl-4-(2-methyl-tetrazol-5-yl)-phenoxy]-propyl]-2,5-dimethoxy-2,5-dihyrofuran.

후처리

  1. customthe resulting reaction mixture
  2. stirringto stir at -10° C. for 45 min
  3. extractionextracted with ether (3×25 mL)
  4. washthe organic layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customto yield an oil which
  8. customwas purified by MPLC chromatography (ethyl acetate/hexane 3:7)

출처 및 근거

ORD 기록
ord-59e3da985c9f435f8506b6e61a2150e6
출처 데이터셋
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05567717

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트