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

HRID 1105716

反応式

HRID 1105716 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f67ddac55063423aa6c6229eb1daa2d8
出典データセット
uspto-grants-1982_01
特許番号
US04309566

関連ノート

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