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

Trifluoroacetic acid → 4-(2-Hydroxyethoxy)-3-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)benzamide

HRID 629073
노트
인쇄 미리보기

반응식

HRID 629073 반응식
Br[C:2]1[CH:3]=[C:4]([CH:19]=[CH:20][C:21]=1[OH:22])[C:5]([NH:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][C:15]([F:18])([F:17])[F:16])=[CH:10][CH:9]=1)=[O:6].C([O:26][CH2:27][CH2:28]Br)(=O)C.C([O-])([O-])=O.[K+].[K+].[N:36]1[CH:41]=[C:40](B(O)O)[CH:39]=[N:38][CH:37]=1.[OH-].[Na+].C(O)(C(F)(F)F)=O>CC(C)=O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.CO.COCCOC.CCO>[OH:26][CH2:27][CH2:28][O:22][C:21]1[CH:20]=[CH:19][C:4]([C:5]([NH:7][C:8]2[CH:13]=[CH:12][C:11]([O:14][C:15]([F:18])([F:17])[F:16])=[CH:10][CH:9]=2)=[O:6])=[CH:3][C:2]=1[C:40]1[CH:41]=[N:36][CH:37]=[N:38][CH:39]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

12

반응물 6

HCID 6422Trifluoroacetic acidHCID 11430Potassium CarbonateHCID 135641-Acetoxy-2-bromoethaneHCID 14798Sodium HydroxideHCID 2795193(Pyrimidin-5-yl)boronic acidHCID 899069273-Bromo-4-hydroxy-N-(4-(trifluoromethoxy)phenyl)benzamide

생성물 1

HCID 72201873
4-(2-Hydroxyethoxy)-3-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)benzamide

시약·촉매·용매 5

HCID 178418476HCID 178418476, 화합물촉매HCID 180Acetone용매HCID 702Ethanol용매HCID 887Methanol용매HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
75 °C

실험 절차

A suspension of 3-bromo-4-hydroxy-N-(4-(trifluoromethoxy)phenyl)benzamide (50 mg, 0.133 mmol), 2-bromoethyl acetate (21.94 μL, 0.199 mmol) and powdered K2CO3 (92 mg, 0.665 mmol) in acetone (500 μL) was stirred at 75° C. for 16 h and the solvent was evaporated off under reduced pressure. The residue, together with pyrimidin-5-ylboronic acid (57.61 mg, 0.465 mmol), Pd(PPh3)2Cl2 (18.66 mg, 0.026 mmol) water (125 μL), EtOH (62 μL) and DME (550 μL) were added to a vial, which was sealed, evacuated/purged with argon and the RM stirred at 80° C. for 20 h. The RM was diluted with THF (3 mL) then stirred with Si-Thiol (Silicycle, 105 mg, 0.133 mmol) for 2 h, filtered and the filtrate was evaporated off under reduced pressure to give the crude product which was purified by flash chromatography (Silica gel column, 12 g, cyclohexane/EtOAc from 30% to 95% EtOAc) to afford the acylated product, which was treated with aq. 4 M NaOH (138 μL, 0.552 mmol) and MeOH (250 μL) at and stirred at RT for 4 h. The RM was acidified with TFA and purified by preparative HPLC (Condition 8, 50% for 0.2 min then 50% to 80% in 14 min) to afford the title compound as a beige solid. UPLC-MS (Condition 1) tR=2.24 min, m/z=420.0 [M+H]+, m/z=418 [M−H]−; 1H-NMR (400 MHz, DMSO-d6) δ ppm 3.64-3.82 (m, 2H) 4.21 (t, J=4.6 Hz, 2H) 4.91 (t, J=5.4 Hz, 1H) 7.32-7.41 (m, 3H) 7.88 (d, J=9.0 Hz, 2H) 8.07 (dd, J=8.8, 2.2 Hz, 1H) 8.12 (d, J=2.2 Hz, 1H) 9.13 (s, 2H) 9.18 (s, 1H) 10.32 (s, 1H).

후처리

  1. customthe solvent was evaporated off under reduced pressure
  2. customwas sealed
  3. customevacuated/purged with argon
  4. stirringthe RM stirred at 80° C. for 20 h
  5. additionThe RM was diluted with THF (3 mL)
  6. filtrationfiltered
  7. customthe filtrate was evaporated off under reduced pressure
  8. customto give the crude product which
  9. customwas purified by flash chromatography (Silica gel column, 12 g, cyclohexane/EtOAc from 30% to 95% EtOAc)
  10. customto afford the acylated product, which
  11. stirringstirred at RT for 4 h
  12. custompurified by preparative HPLC (Condition 8, 50% for 0.2 min

출처 및 근거

ORD 기록
ord-98eb6623127841128289459c820b2b49
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09315489B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트