반응식
[C:1]1([NH2:15])[N:2]=[C:3]([NH2:14])[N:4]=[C:5]2[C:10]=1[C:9]1[CH:11]=[CH:12][NH:13][C:8]=1[CH:7]=[CH:6]2.[H-].[Na+].[CH2:18](Br)[CH:19]1[O:23][CH2:22][CH2:21][CH2:20]1.Cl>CC(C)=O.CN(C)C=O>[O:23]1[CH2:22][CH2:21][CH2:20][CH:19]1[CH2:18][N:13]1[C:8]2[CH:7]=[CH:6][C:5]3[C:10](=[C:1]([NH2:15])[N:2]=[C:3]([NH2:14])[N:4]=3)[C:9]=2[CH:11]=[CH:12]1참가 물질
실험 절차
In a manner similar to that of Example 2, 3.98 g. of 7H-pyrrolo[3,2-f]quinazoline-1,3-diamine in ca. 260 ml. dry dimethylformamide are reacted with 1.06 g. ca. 50% sodium hydride-mineral oil dispersion and then with 3.63 g. tetrahydrofurfuryl bromide. After stirring the mixture at ca. 25° for 24 hours, 0.21 g. ca. 50% sodium hydride-mineral oil dispersion are added. Stirring is continued for one-hour, 0.73 g. tetrahydrofurfuryl bromide is added, and, after stirring for 6 hours, the reaction mixture is kept at ca. 25° for ca. 70 hours. Processing of the reaction mixture in the manner described in Example 2 (Method A) yields a brown gum which is dissolved in 40 ml. N hydrochloric acid. Dilution of the aqueous acidic solution with 40 ml. acetone gives crystals that are collected and twice recrystallized from methanol-acetone to yield 1.20 g. title compound as a monohydrochloride salt bearing one-third molecule of water per molecule of diamine salt, m.p. 310°-311° (dec.).
후처리
- stirringStirring
- waitis continued for one-hour
- stirringafter stirring for 6 hours
- waitthe reaction mixture is kept at ca. 25° for ca. 70 hours
- customyields a brown gum which
- dissolutionis dissolved in 40 ml
- customare collected
- customtwice recrystallized from methanol-acetone
- customto yield 1.20 g
출처 및 근거
- ORD 기록
- ord-ed257ea02bc74b5fbf2aac893c73c79e
- 출처 데이터셋
- uspto-grants-1978_10
- 특허 번호
- US04118561
연결된 노트
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