Hydrochloric Acid → HCID 86609751、化合物

HRID 1710807ノート

反応式

HRID 1710807 の反応式
[BH4-].[Na+].[NH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Cl:10])[C:5]=1[C:11](=O)[CH3:12].[C:14]([S-:16])#[N:15].[K+].Cl>C(O)C.CCCCCCC.C(OCC)(=O)C.O>[Cl:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:4]2[C:5]=1[CH:11]([CH3:12])[NH:15][C:14](=[S:16])[NH:3]2

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 516872Potassium thiocyanateHCID 4311764Sodium borohydrideHCID 228886971-(2-Amino-6-chlorophenyl)ethanone

生成物 1

HCID 86609751HCID 86609751、化合物

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 21899848Ethylacetate heptane溶媒

反応条件

温度
65 °C

実験手順

At a temperature of 65° C., sodium borohydride was added to a solution of 1-(2-amino-6-chloro-phenyl)-ethanone in ethanol, and the mixture was heated overnight (65° C.). Water, KSCN and HCl were then added subsequently, and the mixture was again heated (3 h, 65° C.). The majority of the title compound precipitated upon cooling and could be isolated in sufficiently pure form by filtration. A small additional amount of the desired product was obtained by workup of the mother liquor (evaporation of solvent, column chromatography [silica gel, solvent gradient n-heptan/ethyl acetate=100/0−60/40]). The title compound was obtained in a combined yield of 1.46 g (43%).

後処理

  1. temperaturethe mixture was again heated (3 h, 65° C.)
  2. customThe majority of the title compound precipitated
  3. temperatureupon cooling
  4. customcould be isolated in sufficiently pure form by filtration

出典と根拠

ORDレコード
ord-c9f57a16dd08423cb961f38a6ab4fbab
出典データセット
uspto-grants-2010_09
特許番号
US07790732B2

反応ノート

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