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

Bromine → HCID 21470010, 화합물

HRID 1938813
노트
인쇄 미리보기

반응식

HRID 1938813 반응식
[Br:1]Br.[Cl-].[OH:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[CH:7][C:6]=1[CH2:13][P+:14]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>CO>[Br-:1].[Br:1][C:10]1[C:5]([OH:4])=[C:6]([CH2:13][P+:14]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH:7]=[C:8]([O:11][CH3:12])[CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24408BromineHCID 21470013(2-Hydroxy-5-methoxybenzyl)triphenylphosphonium chloride

생성물 1

HCID 21470010HCID 21470010, 화합물수율 76%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In the course of 1.5 hours, at 5°, 13 g of bromine are added dropwise to a solution of 35 g of [(2-hydroxy-5-methoxy-phenyl)methyl]-triphenyl-phosphonium chloride in 700 ml of methanol. The solution is concentrated in vacuo at 20° to 110 ml, 220 ml of ethyl acetate are added thereto in the course of 2 hours, the resulting yellow suspension is stirred for 2 hours at 0°, and the slightly yellow crystals are filtered off with suction and recrystallised from methanol. A mixture of colourless crystals (m.p.: 210°) which according to AgNO3 titre comprises 22.4 percent by weight [(3-bromo-2-hydroxy-5-methoxy-phenyl)methyl ]-triphenyl-phosphonium chloride and 77.6 percent by weight [(3-bromo-2-hydroxy-5-methoxy-phenyl)methyl]-triphenyl-phosphonium bromide is obtained; yield 76 % of the theoretical yield.

후처리

  1. concentrationThe solution is concentrated in vacuo at 20° to 110 ml, 220 ml of ethyl acetate
  2. additionare added
  3. filtrationthe slightly yellow crystals are filtered off with suction
  4. customrecrystallised from methanol
  5. additionA mixture of colourless crystals (m.p.: 210°) which

출처 및 근거

ORD 기록
ord-fc71f5105c234909a7eefc0505f9ea83
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05693807

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트