반응식
O.[OH-].[Li+].O.C[O:6][C:7]([C:9]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:11]([C:18]2[C:19]3[CH:26]=[CH:25][N:24]([CH3:27])[C:20]=3[N:21]=[CH:22][N:23]=2)[CH:10]=1)=[O:8]>O1CCCC1>[C:7]([C:9]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:11]([C:18]2[C:19]3[CH:26]=[CH:25][N:24]([CH3:27])[C:20]=3[N:21]=[CH:22][N:23]=2)[CH:10]=1)([OH:8])=[O:6]참가 물질
반응 조건
- 온도
- 20 °C
실험 절차
0.629 g (15 mmol) of lithium hydroxide monohydrate and 20 cm3 of water are added to 1.35 g (4.41 mmol) of 3-methoxycarbonyl-1-(7-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-indole dissolved in 20 cm3 of tetrahydrofuran at a temperature in the region of 20° C. After stirring for 4 hours at the reflux temperature of the solvent and for 24 hours at a temperature in the region of 20° C., the reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa). The residue is taken up in 30 cm3 of water (pH=12) and extracted with 100 cm3 of ethyl acetate. The pH is then adjusted to 6 by adding 1 N hydrochloric acid solution. The precipitate obtained is filtered off and dried at a temperature in the region of 50° C. under reduced pressure (2.7 kPa), giving 1.0 g of 3-carboxy-1-(7-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-indole in the form of a white powder. Mass spectrum (EI): m/e 292 (M+) (base peak).
후처리
- concentrationthe reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa)
- extractionextracted with 100 cm3 of ethyl acetate
- additionby adding 1 N hydrochloric acid solution
- customThe precipitate obtained
- filtrationis filtered off
- customdried at a temperature in the region of 50° C. under reduced pressure (2.7 kPa)
출처 및 근거
- ORD 기록
- ord-4c28a474da9c4ad6b7298f492c723a88
- 출처 데이터셋
- uspto-grants-2009_12
- 특허 번호
- US07638521B2
연결된 노트
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