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

Boron trifluoride etherate → Tert-butyl 4-(adamantan-2-yl(hydroxy)methyl)-3-chlorobenzoate

HRID 1849749
노트
인쇄 미리보기

반응식

HRID 1849749 반응식
Br[C:2]1[CH:14]=[CH:13][C:5]([C:6]([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7])=[CH:4][C:3]=1[Cl:15].[Cl-].[Li+].C([Mg]Cl)(C)C.[O:23]1[CH2:25][C:24]21[CH:32]1[CH2:33][CH:28]3[CH2:29][CH:30]([CH2:34][CH:26]2[CH2:27]3)[CH2:31]1.B(F)(F)F.CCOCC>O1CCCC1>[CH:26]12[CH2:34][CH:30]3[CH2:29][CH:28]([CH2:33][CH:32]([CH2:31]3)[CH:24]1[CH:25]([OH:23])[C:2]1[CH:14]=[CH:13][C:5]([C:6]([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7])=[CH:4][C:3]=1[Cl:15])[CH2:27]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8000Boron trifluoride etherateHCID 303804Spiro[adamantane-2,2'-oxirane]HCID 81295241Tert-butyl 4-bromo-3-chlorobenzoateHCID 178461733HCID 178461733, 화합물

생성물 1

HCID 86703631Tert-butyl 4-(adamantan-2-yl(hydroxy)methyl)-3-chlorobenzoate수율 33%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

To a solution of tert-butyl 4-bromo-3-chlorobenzoate (0.875 g, 3.00 mmol) in tetrahydrofuran (5 mL) was added isopropylmagnesium chloride lithium chloride complex (1.3 M solution in anhydrous tetrahydrofuran, 2.78 mL, 3.61 mmol) at −40° C. The reaction was allowed to warm to ambient temperature and stirred for 1 hour (solution A). In a separate flask, a solution of spiro(adamantane-2,2′-oxirane) (0.492 g, 3.00 mmol) in anhydrous tetrahydrofuran (5 mL) was treated with boron trifluoride diethyl etherate (0.38 mL, 3.0 mmol) at 0° C. for 30 minutes (solution B). Solution A was then transferred via cannula to solution B at 0° C. The reaction mixture was allowed to warm to ambient temperature and stirred for 16 hours. After quenched with saturated ammonium chloride solution (5 mL), the mixture was extracted with ethyl acetate (3×10 mL). The combined organic phase was dried over anhydrous sodium sulfate, and filtered. Concentration of the filtrate in vacuo gave a residue which was purified by silica gel column chromatography using 0-100% ethyl acetate in hexanes as eluent to afford the title compound as a colorless solid (0.32 g, 33%): 1H NMR (300 MHz, DMSO-d6) δ 7.84 (dd, J=8.1, 1.4 Hz, 1H), 7.80 (d, J=1.5 Hz, 1H), 7.64 (d, J=8.1 Hz, 1H), 5.44 (br s, 1H), 5.18 (d, J=10.3 Hz, 1H), 2.36-2.29 (m, 1H), 2.06-1.34 (m, 22H), 1.08-1.01 (m, 1H); MS (ES+) m/z 359.2, 361.2 (M−17).

후처리

  1. temperatureto warm to ambient temperature
  2. customAfter quenched with saturated ammonium chloride solution (5 mL)
  3. extractionthe mixture was extracted with ethyl acetate (3×10 mL)
  4. dry with materialThe combined organic phase was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customConcentration of the filtrate in vacuo gave a residue which
  7. customwas purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-914cc75b7c9c48459d2852ae63ddd59d
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08952169B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트