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

HRID 2268266노트

반응식

HRID 2268266 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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-dimethylethy] 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.

후처리

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

출처 및 근거

ORD 기록
ord-facdcf5c2b0f4699ad304b55f03ace57
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06326500B1

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