Hydrochloric Acid → HCID 15087823, 화합물

HRID 1073181노트

반응식

HRID 1073181 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([NH:9][C:10](=[O:12])[CH3:11])=[C:4]([Cl:13])[CH:3]=1.S1C=[CH:17][CH:16]=[CH:15]1.[F-].[K+].Cl.[H][H]>CO.[Pt].CC(O)C.CC(=O)C>[Cl:13][C:4]1[CH:3]=[C:2]([NH:1][CH:16]([CH3:17])[CH3:15])[CH:7]=[C:6]([Cl:8])[C:5]=1[NH:9][C:10](=[O:12])[CH3:11]

참가 물질

10

반응물 5

HCID 313Hydrochloric AcidHCID 8030ThiopheneHCID 256806N-(4-Amino-2,6-dichlorophenyl)ethanimidic acidHCID 522689Potassium FluorideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 15087823HCID 15087823, 화합물수율 66.7%

시약·촉매·용매 4

HCID 23939Platinum촉매HCID 180Acetone용매HCID 887Methanol용매2회HCID 3776Isopropanol용매

실험 절차

A mixture of 20 parts of N-(4-amino-2,6-dichlorophenyl)acetamide, 10 parts of 2-propanone, 2 parts of a solution of thiophene in methanol 4%, 400 parts of methanol, 5 parts of potassium fluoride and 18 parts of 2-propanol, saturated with hydrogen chloride was hydrogenated in a Parr apparatus and at 50° C. with 2 parts of platinum-on-charcoal catalyst 5%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated. The residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 15.7 parts (66.7%) of N-[2,6-dichloro-4-[(1-methylethyl)amino]phenyl]acetamide (int. 98).

후처리

  1. filtrationthe catalyst was filtered off
  2. customthe filtrate was evaporated
  3. customThe residue was crystallized from acetonitrile
  4. filtrationThe product was filtered off
  5. customdried

출처 및 근거

ORD 기록
ord-c429f1bf49c140dab93c83a8a7f98366
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04968684

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