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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethyl formate → 1-(3'-Aminophenyl)-2-formylamino-propane

HRID 614872
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인쇄 미리보기

반응식

HRID 614872 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH2:8][CH:9]([NH2:11])[CH3:10])[CH:5]=[CH:6][CH:7]=1.[CH:12](OCC)=[O:13]>>[NH2:1][C:2]1[CH:3]=[C:4]([CH2:8][CH:9]([NH:11][CH:12]=[O:13])[CH3:10])[CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 8025Ethyl formateHCID 204423703-(2-Aminopropyl)aniline

생성물 1

HCID 213274251-(3'-Aminophenyl)-2-formylamino-propane

실험 절차

A mixture of 1-(3'-amino-phenyl)-2-amino-propane and12.5 ml of ethyl formate was boiled for ten hours, and then the reaction mixture was evaporated, leaving 1-(3'-aminophenyl)-2-(formyl-amino)-propane. 4.45 gm of this amide were dissolved in 25 ml of pyridine, 2.6 ml of chlorothioformic acid-S-ethyl ester were added to the solution at 10-20° C., and the mixture was allowed to stand for a few hours. Therefore, the reaction solution was poured into ice water, and the aqueous mixture was extracted with ether. The ethereal extract was washed five times with water and once briefly with 1/10 N hydrochloric acid, and was then evaporated, leaving as a residue 1-[3'-(ethylthiocarbonyl-amino)-phenyl]-2-(formyl-amino)-propane. The residue was added to a mixture of 75 ml of methanol and 5 ml of concentrated hydrochloric acid, and the mixture was allowed to stand for three days at room temperature. Thereafter, the resulting solution was evaporated, the residue was triturated with acetonitrile, and the crystalline product formed thereby was recrystallized from acetonitrile and a little water, yielding the hydrochloride of the formula ##STR19## which has a melting point of 185°-186° C.

후처리

  1. customthe reaction mixture was evaporated

출처 및 근거

ORD 기록
ord-4981b306caed4b1cbf23600217f28718
출처 데이터셋
uspto-grants-1979_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04146645

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