Hydrochloric Acid → N-(4-Fluoro-3-chloro-phenyl)-2-[N-methyl-N-(2,2-difluoroethyl)-amino]-4-methylamino-5-nitro-benzoic acid amide

HRID 1189633노트

반응식

HRID 1189633 반응식
[F:1][CH:2]([F:6])[CH2:3][NH:4][CH3:5].Cl.CCN(C(C)C)C(C)C.[F:17][C:18]1[CH:23]=[CH:22][C:21]([NH:24][C:25](=[O:38])[C:26]2[CH:31]=[C:30]([N+:32]([O-:34])=[O:33])[C:29]([NH:35][CH3:36])=[CH:28][C:27]=2F)=[CH:20][C:19]=1[Cl:39]>CC#N>[F:17][C:18]1[CH:23]=[CH:22][C:21]([NH:24][C:25](=[O:38])[C:26]2[CH:31]=[C:30]([N+:32]([O-:34])=[O:33])[C:29]([NH:35][CH3:36])=[CH:28][C:27]=2[N:4]([CH3:5])[CH2:3][CH:2]([F:6])[F:1])=[CH:20][C:19]=1[Cl:39]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 81531DiisopropylethylamineHCID 233232502,2-difluoro-N-methylethanamineHCID 67957648N-(4-Fluoro-3-chloro-phenyl)-2-fluoro-4-methylamino-5-nitro-benzoic acid amide

생성물 1

HCID 86666463N-(4-Fluoro-3-chloro-phenyl)-2-[N-methyl-N-(2,2-difluoroethyl)-amino]-4-methylamino-5-nitro-benzoic acid amide

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of N-(2,2-difluoroethyl)-N-methyl-amine×HCl (64 mg, 0.48 mmol), DIPEA (0.64 ml, 3.73 mmol), N-(4-fluoro-3-chloro-phenyl)-2-fluoro-4-methylamino-5-nitro-benzoic acid amide (150 mg, 0.44 mmol) and MeCN (5 mL) is stirred for two weeks at reflux. Then the mixture is concentrated, diluted with EtOAc, washed with water, dried with Na2SO4 and concentrated and directly used in the next step.

후처리

  1. temperatureat reflux
  2. concentrationThen the mixture is concentrated
  3. additiondiluted with EtOAc
  4. washwashed with water
  5. dry with materialdried with Na2SO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-95e76a4fbdac4df9a635710c329bcbf1
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08674113B2

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