2,3,6-Trichlorobenzoic acid → (Aminocarbonyl)Methyl 2,3,6-Trichlorobenzoate

HRID 1105716

반응식

HRID 1105716 반응식
[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][CH:8]=[C:7]([Cl:12])[C:3]=1[C:4]([OH:6])=[O:5].[OH-].[K+].Cl[CH2:16][C:17]([NH2:19])=[O:18].O1CCOCCOCCOCCOCCOCC1>C1(C)C=CC=CC=1.CN(C)C=O>[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][CH:8]=[C:7]([Cl:12])[C:3]=1[C:4]([O:6][CH2:16][C:17]([NH2:19])=[O:18])=[O:5]

참가 물질

7

반응물 4

HCID 57592,3,6-Trichlorobenzoic acidHCID 6580ChloroacetamideHCID 14797Potassium HydroxideHCID 2855718-Crown-6

생성물 1

HCID 2417794(Aminocarbonyl)Methyl 2,3,6-Trichlorobenzoate

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6228Dimethylformamide용매

실험 절차

This compound was prepared in the manner of Example I, using 15.0 grams (0.066 mole) of 2,3,6-trichlorobenzoic acid, 4.4 grams (0.066 mole) of potassium hydroxide, 6.2 grams (0.066 mole) of 2-chloroacetamide, and 1.8 grams of 1,4,7,10,13,16-hexaoxacyclooctadecane in 300 ml of dry toluene and 200 ml of dimethylformamide. The crude product was purified by liquid chromatography, followed by recrystallization from ethyl acetate. The yield was 0.9 gram of (aminocarbonyl)methyl 2,3,6-trichlorobenzoate; mp 158°-160°. The ir and the nmr spectra were consistent with the proposed structure.

후처리

  1. customThis compound was prepared in the manner of Example I
  2. customThe crude product was purified by liquid chromatography
  3. customfollowed by recrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-f67ddac55063423aa6c6229eb1daa2d8
출처 데이터셋
uspto-grants-1982_01
특허 번호
US04309566

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