Hydrochloric Acid → HCID 54511686, 화합물

HRID 1387530노트

반응식

HRID 1387530 반응식
Cl.[CH3:2][O:3][C:4](=[O:25])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[C:7]([N:13](C(=O)C)[C:14]2[CH:19]=[C:18]([Cl:20])[CH:17]=[C:16]([Cl:21])[CH:15]=2)[CH:6]=1>O1CCCC1.CO>[CH3:2][O:3][C:4](=[O:25])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[C:7]([NH:13][C:14]2[CH:19]=[C:18]([Cl:20])[CH:17]=[C:16]([Cl:21])[CH:15]=2)[CH:6]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 543001583-[Acetyl-(3,5-dichlorophenyl)-amino]-4-methoxybenzoic acid methyl ester

생성물 1

HCID 54511686HCID 54511686, 화합물수율 23.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

Concentrated HCl (45 mL) was added to a solution of 3-[acetyl-(3,5-dichlorophenyl)-amino]-4-methoxybenzoic acid methyl ester (11.46 g, 31.12 mmol) in a mixture of tetrahydrofuran (75 mL) and methanol (75 mL). The reaction was heated to reflux. After 3 days, the solvent was removed in vacuo and the residue was dissolved in ethyl acetate and dried (MgSO4). The ethyl acetate was removed under reduced pressure to give the product (2.4 g); m.p. 134-135° C. after chromatography on silica gel in ethyl acetate followed by recrystallization from ether/hexane 1:9.

후처리

  1. temperatureThe reaction was heated to reflux
  2. customthe solvent was removed in vacuo
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. dry with materialdried (MgSO4)
  5. customThe ethyl acetate was removed under reduced pressure

출처 및 근거

ORD 기록
ord-82a32adeb35345acbbd2ecd0eefd25fa
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06268387B1

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