Triethylamine → HCID 18975624, 화합물

HRID 2393329노트

반응식

HRID 2393329 반응식
[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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 900213-Chloro-6-isothiocyanatotolueneHCID 12227201HCID 12227201, 화합물

생성물 1

HCID 18975624HCID 18975624, 화합물수율 36.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

출처 및 근거

ORD 기록
ord-a14f1ca3b07549ada6682576dd54aa71
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05807864

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