Hydrochloric Acid → HCID 15087823、化合物

HRID 1073181ノート

反応式

HRID 1073181 の反応式
[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]

参加物

10

反応物 5

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

生成物 1

HCID 15087823HCID 15087823、化合物収率 66.7%

試薬・触媒・溶媒 4

HCID 23939Platinum触媒HCID 180Acetone溶媒HCID 887Methanol溶媒2 回HCID 3776Isopropanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c429f1bf49c140dab93c83a8a7f98366
出典データセット
uspto-grants-1990_11
特許番号
US04968684

反応ノート

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