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

3-Fluoro-4-hydroxybenzaldehyde → 4-[3-(Biphenyl-4-yloxy)-propoxy]-3-fluoro-benzaldehyde

HRID 459159
노트
인쇄 미리보기

반응식

HRID 459159 반응식
CC(C)([O-])C.[K+].[F:7][C:8]1[CH:9]=[C:10]([CH:13]=[CH:14][C:15]=1[OH:16])[CH:11]=[O:12].Br[CH2:18][CH2:19][CH2:20][O:21][C:22]1[CH:27]=[CH:26][C:25]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)=[CH:24][CH:23]=1>CN(C)C=O.O>[C:25]1([C:28]2[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=2)[CH:24]=[CH:23][C:22]([O:21][CH2:20][CH2:19][CH2:18][O:16][C:15]2[CH:14]=[CH:13][C:10]([CH:11]=[O:12])=[CH:9][C:8]=2[F:7])=[CH:27][CH:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 5872503-Fluoro-4-hydroxybenzaldehydeHCID 152334631,1'-Biphenyl, 4-(3-bromopropoxy)-HCID 23665647Potassium tert-butoxide

생성물 1

HCID 184436794-[3-(Biphenyl-4-yloxy)-propoxy]-3-fluoro-benzaldehyde수율 83.2%

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매

실험 절차

Potassium tert-butoxide (198 mg, 1.76 mmol) was added, at 0° C., to a solution of 3-Fluoro-4-hydroxy-benzaldehyde (235 mg, 1.68 mmol) in dry N,N-dimethylformamide (2 mL). The mixture was stirred for 10 minutes. 4-(3-Bromo-propoxy)-biphenyl (example 23, Step D) (539 mg, 1.84 mmol) was added and the reaction was stirred for 24 hours at room temperature. The mixture was diluted with water (15 mL) and extracted with ethyl acetate (4×15 mL). The combined organic layers were dried (Na2SO4), filtered, and concentrated under vacuum to produce a solid which was washed with hexanes to produce 4-[3-(Biphenyl-4-yloxy)-propoxy]-3-fluoro-benzaldehyde as a pale brown solid (490 mg, 83%). 1H-NMR (CDCl3, 200.15 MHz): δ 9.83 (d, 1H, J=2.2), 7.64–7.23 (m, 9H), 7.09 (t, 1H, J=8.2), 6.96 (d, 2H, J=8.8), 4.32 (t, 2H, J=5.9), 4.21 (t, 2H, J=5.9), 2.35 (qn, 2H, J=5.9).

후처리

  1. stirringthe reaction was stirred for 24 hours at room temperature
  2. extractionextracted with ethyl acetate (4×15 mL)
  3. dry with materialThe combined organic layers were dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum
  6. customto produce a solid which
  7. washwas washed with hexanes

출처 및 근거

ORD 기록
ord-d0726478f142444396bab02c57ecc530
출처 데이터셋
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07192982B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트