Triethylamine → HCID 18975624、化合物

HRID 2393329ノート

反応式

HRID 2393329 の反応式
[CH2:1]([NH:3][CH2:4][CH2:5][C:6]([OH:8])=[O:7])[CH3:2].[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([N:16]=[C:17]=[S:18])=[C:12]([CH3:19])[CH:11]=1.C(N(CC)CC)C>C(Cl)Cl>[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([NH:16][C:17](=[S:18])[N:3]([CH2:4][CH2:5][C:6]([OH:8])=[O:7])[CH2:1][CH3:2])=[C:12]([CH3:19])[CH:11]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 900213-Chloro-6-isothiocyanatotolueneHCID 12227201HCID 12227201、化合物

生成物 1

HCID 18975624HCID 18975624、化合物収率 36.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3-Ethylaminopropionic acid (19.8 g) was reacted with 4-chloro-2-methylphenylisothiocyanate (20 g), triethylamine (20 g), and methylene chloride (250 mL) according to the procedure described in step 2 of Example 1 to give 12 g of 3-[3-(4-chloro-2-methylphenyl)-1-ethyl-thioureido]propionic acid. The product (12 g) was dissolved in acetone (245 mL). Conc. HCl (5 mL) was added and the mixture was heated at reflux for 18 hours. The reaction mixture was evaporated to dryness. The residue was dissolved in methylene chloride (100 mL), and washed with 1N NaOH. The organic phase was dried over anhydrous magnesium sulfate, then evaporated to dryness. The solid was recrystallized from ethanol. The title compound (8 g) was obtained as a white solid., m.p. 133°-136° C.

出典と根拠

ORDレコード
ord-a14f1ca3b07549ada6682576dd54aa71
出典データセット
uspto-grants-1998_09
特許番号
US05807864

反応ノート

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