Sulfuric Acid → 8-chloro-1-ethyl-6-phenyl-4H-s-triazolo-[4,3-a][1,4]benzodiazepine

HRID 1764522

반응식

HRID 1764522 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([NH:12][NH2:13])[CH2:9][N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]=2[CH:20]=1.[C:21]([O-])([O-])(OCC)[CH2:22][CH3:23].S(=O)(=O)(O)O>C(O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[C:21]([CH2:22][CH3:23])=[N:13][N:12]=[C:10]3[CH2:9][N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]=2[CH:20]=1

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 123908747-Chloro-2-hydrazinyl-5-phenyl-3H-1,4-benzodiazepineHCID 86600181Ethyl ortho-propionate

생성물 1

HCID 125606218-chloro-1-ethyl-6-phenyl-4H-s-triazolo-[4,3-a][1,4]benzodiazepine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a mixture of 1.4 parts of 7-chloro-2-hydrazino-5-phenyl-3H-1,4-benzodiazepine prepared in Example 1, 50 parts by volume of ethanol and 4 parts by volume of ethyl orthopropionate is added 0.5 part by volume of concentrated sulfuric acid. The mixture is stirred for 30 minutes at room temperature and then treated in a similar manner to Example 14, whereby 8-chloro-1-ethyl-6-phenyl-4H-s-triazolo- [4,3-a] [1,4] benzodiazepine is yielded as crystals. Recrystallization from acetone yields colorless prisms melting at 229° C to 230° C.

후처리

  1. additiontreated in a similar manner to Example 14

출처 및 근거

ORD 기록
ord-2c0ce17b698b48afa29b45cdace682b9
출처 데이터셋
uspto-grants-1978_09
특허 번호
US04116956

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