N,N-Dimethylbenzylamine → 4,4'-Dibromostilbene

HRID 1156252

반응식

HRID 1156252 반응식
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=O)=[CH:4][CH:3]=1.[Br:11][C:12]1[CH:19]=[CH:18][C:15]([CH:16]=C)=[CH:14][CH:13]=1.C(N(C)C)C1C=CC=CC=1>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.CC1C=CC=CC=1C>[Br:1][C:2]1[CH:10]=[CH:9][C:5]([CH:6]=[CH:16][C:15]2[CH:18]=[CH:19][C:12]([Br:11])=[CH:13][CH:14]=2)=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 7681N,N-DimethylbenzylamineHCID 162634-BromostyreneHCID 685154-Bromobenzoyl chloride

생성물 1

HCID 533959814,4'-Dibromostilbene수율 46.1%

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 7237O-Xylene용매

실험 절차

0.112 mg (0.5 millimols) of palladium acetate, 10.97 g (50 millimols) of 4-bromobenzoyl chloride, 10.17 g (50 millimols) of 4-bromostyrene and 6.76 g (50 millimols) of N-benzyldimethylamine in 100 m of o-xylene are stirred for 1 hour at 130° C. After having filtered off the amine salt which has precipitated, the filtrate is concentrated and the crude product is recrystallised twice from toluene. 7.8 g (46% of theory) of 4,4'-dibromostilbene are obtained in the form of white flakes; melting point 213.3° C.

후처리

  1. filtrationAfter having filtered off the amine salt which
  2. customhas precipitated
  3. concentrationthe filtrate is concentrated
  4. customthe crude product is recrystallised twice from toluene

출처 및 근거

ORD 기록
ord-32cec8b9af47431d904cd532230fa04b
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04335055

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