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

Zinc → HCID 178497614, 화합물

HRID 612440
노트
인쇄 미리보기

반응식

HRID 612440 반응식
[Zn:1].[Br:2]C[C:4]1[CH:5]=[C:6]([C:16]([O:18][CH3:19])=[O:17])[C:7](C2C=CC=CC=2)=[CH:8][CH:9]=1.ClC1C2C(=CC=CC=2)N=[C:23]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)N=1>O1CCCC1>[Br-:2].[CH3:19][O:18][C:16]([C:6]1[CH:7]=[CH:8][CH:9]=[CH:4][C:5]=1[C:34]1[CH:33]=[CH:32][C:31]([CH2:23][Zn+:1])=[CH:36][CH:35]=1)=[O:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 23994ZincHCID 809774-Chloro-2-phenylquinazolineHCID 19595328Methyl 4-(bromomethyl)(1,1'-biphenyl)-2-carboxylate

생성물 1

HCID 178497614HCID 178497614, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

[[2'-(methoxycarbonyl)(1,1'-biphenyl)-4-yl]-methyl] zinc bromide was prepared in advance from 400 mg of zinc in 1 ml of tetrahydrofuran and 1.53 g of methyl 4-(bromomethyl)(1,1'-biphenyl)-2-carboxylate (KNOCHEL, J. Org. Chem., 1988, Vo. 53, p. 5789 to 5791) and 240.69 mg of 4-chloro-2-phenyl-quinazoline and 115 mg of palladium tetrakis(triphenyl-phosphine) complex were added to the solution. The mixture stood at 50° C. for 6 hours and the reaction medium was poured into a water/ice/acetic acid mixture. The aqueous phase was extracted with ethyl acetate and the organic phase was washed with water and water saturated with sodium chloride, dried and evaporated. After chromatography on silica (eluant: ethyl acetate-hexane 1-9 then 2-8), 260 mg of expected product melting at 120° C. to 121° C. after crystallization from isopropyl ether were obtained.

후처리

  1. additionwere added to the solution
  2. extractionThe aqueous phase was extracted with ethyl acetate
  3. washthe organic phase was washed with water and water saturated with sodium chloride
  4. customdried
  5. customevaporated
  6. customAfter chromatography on silica (eluant: ethyl acetate-hexane 1-9 then 2-8), 260 mg of expected product melting at 120° C. to 121° C. after crystallization from isopropyl ether
  7. customwere obtained

출처 및 근거

ORD 기록
ord-fcdcd887dd2f417ab9e58dd5714537e6
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06004979

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트