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2-Methyl-2-butene → HCID 178440015, 화합물

HRID 1708421
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HRID 1708421 반응식
[CH2:1]([C:4]1[N:9]=[C:8]([CH2:10]COC)[N:7]2[NH:14][C:15](=[O:17])[N:16]=[C:6]2[C:5]=1[CH2:18][C:19]1[CH:24]=[CH:23][C:22]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[C:31]2[NH:35][N:34]=[N:33][N:32]=2)=[CH:21][CH:20]=1)[CH2:2][CH3:3].CC=C(C)C.B(Br)(Br)[Br:42]>C(Cl)(Cl)Cl>[CH2:1]([C:4]1[N:9]=[C:8]([CH2:10][Br:42])[N:7]2[NH:14][C:15](=[O:17])[N:16]=[C:6]2[C:5]=1[CH2:18][C:19]1[CH:24]=[CH:23][C:22]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[C:31]2[NH:35][N:34]=[N:33][N:32]=2)=[CH:21][CH:20]=1)[CH2:2][CH3:3]
참가 물질실험 절차출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 105532-Methyl-2-buteneHCID 25134Boron tribromideHCID 178440100HCID 178440100, 화합물

생성물 1

HCID 178440015HCID 178440015, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

1 g of 7-n-propyl-5-methoxyethyl-8-{[2 '- (5-tetrazolyl)-4-biphenylyl]methyl}-1,2,4-triazolo[1,5-c]pyrimidin-2 (3H) -one, prepared in Example 169, are dissolved in 50 ml of chloroform stabilised with amylene. 0.7 ml of boron tribromide is added and the mixture is stirred for 8 hours at room temperature; the derivative 7-n-propyl-5-bromomethyl-8-{[2 '- (5-tetrazolyl ) -4-biphenylyl]methyl}-1,2,4-triazolo[1,5-c]pyrimidin-2(3H )-one thereby formed is taken up with dilute sodium hydroxide solution and stirred again for 6 hours. The aqueous phase is then separated after settling has taken place and acidified by bubbling in sulphur dioxide, and the crystals formed are drained, washed with acetone and then dried to give 0.6 g of 7-n-Propyl-5-hydroxymethyl-8-{[2'-(5 -tetrazolyl ) - 4 -biphenylyl ]methyl }- 1,2,4 -triazolo [ 1,5-c]pyrimidin-2(3H)-one in the form of crystals of melting point 182°-183° C.

출처 및 근거

ORD 기록
ord-d58bd3b2f8d5458f81ad41af3da4400c
출처 데이터셋
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05358950

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