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Bromine → HCID 21470010, 화합물

HRID 486284
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HRID 486284 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
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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-7bde6aab27ce4c938890b3b645768882
출처 데이터셋
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05290939

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