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7-Chloro-2-hydrazinyl-5-phenyl-3H-1,4-benzodiazepine → HCID 53749252, 화합물

HRID 328386
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HRID 328386 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.Cl.[CH2:22]([N:24]([CH2:33][CH3:34])[CH2:25][CH2:26][CH2:27][C:28](=O)[C:29]([OH:31])=[O:30])[CH3:23]>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([NH:12][N:13]=[C:28]([C:29]([OH:31])=[O:30])[CH2:27][CH2:26][CH2:25][N:24]([CH2:33][CH3:34])[CH2:22][CH3:23])[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
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참가 물질

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반응물 2

HCID 123908747-Chloro-2-hydrazinyl-5-phenyl-3H-1,4-benzodiazepineHCID 131710708HCID 131710708, 화합물

생성물 1

HCID 53749252HCID 53749252, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a stirred solution of 2.85 g. (0.01 mole) of 7-chloro-2-hydrazino-5-phenyl-3H-1,4-benzodiazepine in 100 ml. of methanol is added 2.24 g. (0.01 mole) of 5-(diethylamino)-2-oxo-valeric acid, hydrochloride [prepared by the method of Libman and Kutznetsov J. Gen. Chem. (USSR), 33, 1938 (1963)]. The mixture is kept under nitrogen at ambient temperature for 2 hours and then concentrated in vacuo. The residue is mixed with aqueous sodium bicarbonate and extracted with methylene chloride. The extract was washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue of 7-chloro-2-[[1-carboxy-4-(diethylamino)-butylidene]hydrazino]-5-phenyl-3H-1,4-benzodiazepine is used without further purification.

후처리

  1. concentrationconcentrated in vacuo
  2. additionThe residue is mixed with aqueous sodium bicarbonate
  3. extractionextracted with methylene chloride
  4. washThe extract was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue of 7-chloro-2-[[1-carboxy-4-(diethylamino)-butylidene]hydrazino]-5-phenyl-3H-1,4-benzodiazepine is used without further purification

출처 및 근거

ORD 기록
ord-6c64648af2104185bb082a2f0ef3b944
출처 데이터셋
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04017492

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