반응식
S(Cl)([Cl:3])=O.[NH2:5][CH2:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=1.[CH3:16]O>>[ClH:3].[NH2:5][CH2:6][C:7]1[CH:8]=[CH:9][C:10]([C:11]([O:13][CH3:16])=[O:12])=[CH:14][CH:15]=1참가 물질
반응 조건
- 온도
- -30 °C
실험 절차
3.3 cm3 of thionyl chloride are added over 10 minutes to 30 cm3 of methanol cooled to a temperature in the region of -30° C. Stirring is maintained for 30 minutes at a temperature in the region of -23° C. and then 4.7 g of 4-aminomethylbenzoic acid are added. The mixture is left to return to a temperature in the region of 20° C. over 1 hour. The mixture is treated with 15 cm3 of methanol and stirring is maintained for 15 hours at a temperature in the region of 20° C. The solid is separated by filtration, rinsed with a total of 90 cm3 of methanol and then with a total of 150 cm3 of diethyl ether. The solid is dried under reduced pressure (13.5 Pa) at a temperature in the region of 20° C. 3.2 g of methyl 4-aminomethylbenzoate hydrochloride are thus obtained in the form of a white solid melting at a temperature in the region of 270° C.
후처리
- temperatureis maintained for 30 minutes at a temperature in the region of -23° C.
- waitThe mixture is left
- stirringstirring
- temperatureis maintained for 15 hours at a temperature in the region of 20° C
- customThe solid is separated by filtration
- washrinsed with a total of 90 cm3 of methanol
- customThe solid is dried under reduced pressure (13.5 Pa) at a temperature in the region of 20° C
출처 및 근거
- ORD 기록
- ord-c1f2689f3d6e404dbe56ad3975977d0d
- 출처 데이터셋
- uspto-grants-1995_11
- 특허 번호
- US05468888
연결된 노트
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