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1,2-Dichloroethane → Methyl 2'-(((2,4'-dichloro-[1,1'-biphenyl]-4-yl)amino)methyl)-3'-methoxy-5'-(trifluoromethyl)-[1,1'-biphenyl]-4-carboxylate

HRID 2167147
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인쇄 미리보기

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HRID 2167147 반응식
ClCCCl.[CH:5]([C:7]1[C:12]([O:13][CH3:14])=[CH:11][C:10]([C:15]([F:18])([F:17])[F:16])=[CH:9][C:8]=1[C:19]1[CH:24]=[CH:23][C:22]([C:25]([O:27][CH3:28])=[O:26])=[CH:21][CH:20]=1)=O.[Cl:29][C:30]1[CH:35]=[C:34]([NH2:36])[CH:33]=[CH:32][C:31]=1[C:37]1[CH:42]=[CH:41][C:40]([Cl:43])=[CH:39][CH:38]=1>C(Cl)Cl>[Cl:29][C:30]1[CH:35]=[C:34]([NH:36][CH2:5][C:7]2[C:12]([O:13][CH3:14])=[CH:11][C:10]([C:15]([F:16])([F:17])[F:18])=[CH:9][C:8]=2[C:19]2[CH:24]=[CH:23][C:22]([C:25]([O:27][CH3:28])=[O:26])=[CH:21][CH:20]=2)[CH:33]=[CH:32][C:31]=1[C:37]1[CH:42]=[CH:41][C:40]([Cl:43])=[CH:39][CH:38]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 111,2-DichloroethaneHCID 198789103-Chloro-4-(4-chlorophenyl)benzenamineHCID 86674212Methyl 2'-formyl-3'-methoxy-5'-(trifluoromethyl)-[1,1'-biphenyl]-4-carboxylate

생성물 1

HCID 71059990Methyl 2'-(((2,4'-dichloro-[1,1'-biphenyl]-4-yl)amino)methyl)-3'-methoxy-5'-(trifluoromethyl)-[1,1'-biphenyl]-4-carboxylate

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

Solid NaBH(Oac)3 (113 mg, 0.54 mmol) was added to a DCE solution (4 mL) of methyl 2′-formyl-3′-methoxy-5′-(trifluoromethyl)-[1,1′-biphenyl]-4-carboxylate (121 mg, 0.36 mmol) and 2,4′-dichloro-[1,1′-biphenyl]-4-amine (93 mg, 0.39 mmol), and the resulting mixture was stirred at room temperature. After 16 h the resulting mixture was diluted with DCM, washed with saturated aqueous NaHCO3 and water, dried (Na2SO4), concentrated and purified via column chromatography to yield the title compound.

후처리

  1. washwashed with saturated aqueous NaHCO3 and water
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated
  4. custompurified via column chromatography

출처 및 근거

ORD 기록
ord-25e58d3df4c943e6932f2a445852d51d
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09045389B2

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