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Water → Methyl 4-(allylamino)-3-fluoro-2-(2-fluoro-4-iodophenylamino)-5-nitrobenzoate

HRID 1373195
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HRID 1373195 반응식
[CH3:1][O:2][C:3](=[O:24])[C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[C:7](F)=[C:6]([F:14])[C:5]=1[NH:15][C:16]1[CH:21]=[CH:20][C:19]([I:22])=[CH:18][C:17]=1[F:23].O1CCCC1.O.[CH2:31]([NH2:34])[CH:32]=[CH2:33]>CO.C(Cl)Cl>[CH3:1][O:2][C:3](=[O:24])[C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[C:7]([NH:34][CH2:31][CH:32]=[CH2:33])=[C:6]([F:14])[C:5]=1[NH:15][C:16]1[CH:21]=[CH:20][C:19]([I:22])=[CH:18][C:17]=1[F:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 7853AllylamineHCID 8028TetrahydrofuranHCID 58781115Methyl 3,4-difluoro-2-((2-fluoro-4-iodophenyl)amino)-5-nitrobenzoate

생성물 1

HCID 58781109Methyl 4-(allylamino)-3-fluoro-2-(2-fluoro-4-iodophenylamino)-5-nitrobenzoate

시약·촉매·용매 2

HCID 887
Methanol
용매
2회
HCID 6344Dichloromethane용매

실험 절차

A suspension of 3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-5-nitro-benzoic acid methyl ester (456.0 g, 1.008 mol) in a mixture of methanol (4.5 L), tetrahydrofuran (4.5 L) and water (1.13 L) was treated with allylamine (441.89 ml, 336.25 g, 5.88 mol) and stirred at room temperature for 30 min. (completion of reaction was confirmed by TLC-DCM:MeOH/9:1). The yellow colored suspension was filtered and washed with hexane to remove unreacted allylamine and dried to give the title compound as solid (yellow). Yield: 350g (50.90%), mp. 153–154° C.

후처리

  1. filtrationThe yellow colored suspension was filtered
  2. washwashed with hexane
  3. customto remove unreacted allylamine
  4. customdried

출처 및 근거

ORD 기록
ord-7a7ce787382b446d9d622df419439d78
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07160915B2

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