Propionic Acid → N-[2-(4-chloro-2,5-xylylthio)-1,1-dimethylethyl]propionamide

HRID 1956875ノート

反応式

HRID 1956875 の反応式
[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([SH:9])=[C:4]([CH3:10])[CH:3]=1.[NH2:11][C:12]([CH3:16])([CH3:15])[CH2:13]O.[C:17](O)(=[O:20])[CH2:18][CH3:19]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([S:9][CH2:13][C:12]([NH:11][C:17](=[O:20])[CH2:18][CH3:19])([CH3:16])[CH3:15])=[C:4]([CH3:10])[CH:3]=1

参加物

5

反応物 3

HCID 1032Propionic AcidHCID 118072-Amino-2-methyl-1-propanolHCID 1088624-Chloro-2,5-dimethylbenzenethiol

生成物 1

HCID 22007459N-[2-(4-chloro-2,5-xylylthio)-1,1-dimethylethyl]propionamide

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 4-chloro-2,5-dimethylbenzenethiol (17.25 g), 2-amino-2-methylpropanol (8.9 g), propionic acid (7.4 g) and toluene (50 ml) was reacted to give a solid which was recrystallised from petroleum ether, b.p. 60°-80° C. to give N-[2-(4-chloro-2,5-xylylthio)-1,1-dimethylethyl]propionamide, m.p. 78°-81° C. This product (15.0 g) and concentrated hydrochloric acid (18 ml) were boiled under reflux for 25 hours give an oil which was purified by flash column chromatography on silica using ethyl acetate and then ethyl acetate/methanol (4:1) as the mobile phase to give 2-(4-chloro-2,5-xylylthio)-1,1-dimethylethylamine as an oil.

後処理

  1. customwas reacted
  2. customto give a solid which
  3. customwas recrystallised from petroleum ether, b.p. 60°-80° C.

出典と根拠

ORDレコード
ord-a4f61cd137bb4770bd71ff7a2c6f4a44
出典データセット
uspto-grants-1998_07
特許番号
US05780642

反応ノート

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