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Water → 7-chloro-3-[3-(cyclopropyl-methoxy)-1-propynyl]-4,5-dihydro-5 methyl6H-imidazo-[1,5-a][1,4]benzodiazepin-6-one

HRID 1493121
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HRID 1493121 반응식
[OH-].[K+].[Cl:3][C:4]1[C:9]2[C:10](=[O:23])[N:11]([CH3:22])[CH2:12][C:13]3[N:14]([CH:15]=[N:16][C:17]=3[C:18]#[C:19][CH2:20][OH:21])[C:8]=2[CH:7]=[CH:6][CH:5]=1.Br[CH2:25][CH:26]1[CH2:28][CH2:27]1.O>CN(C)C=O>[Cl:3][C:4]1[C:9]2[C:10](=[O:23])[N:11]([CH3:22])[CH2:12][C:13]3[N:14]([CH:15]=[N:16][C:17]=3[C:18]#[C:19][CH2:20][O:21][CH2:25][CH:26]3[CH2:28][CH2:27]3)[C:8]=2[CH:7]=[CH:6][CH:5]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 14797Potassium HydroxideHCID 81503BromomethylcyclopropaneHCID 100405557-chloro-4,5-dihydro-3-(3-hydroxy-1-propynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

생성물 1

HCID 100437977-chloro-3-[3-(cyclopropyl-methoxy)-1-propynyl]-4,5-dihydro-5 methyl6H-imidazo-[1,5-a][1,4]benzodiazepin-6-one수율 85.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3.34 g (59 mmol) of freshly powdered potassium hydroxide were suspended in 25 ml of N,N-dimethylformamide and treated with 4.0 g (13.2 mmol) of 7-chloro-4,5-dihydro-3-(3-hydroxy-1-propynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one. After stirring at room temperature for 5 minutes the mixture was cooled to 2°, whereupon 4.95 g (31.1 mmol) of bromomethylcyclopropane were added thereto. The reaction mixture was stirred at room temperature for 1 hour and then poured into water. The mixture was extracted three times with methylene chloride, the combined organic extracts were washed with water, dried over magnesium sulfate and evaporated. By crystallization of the residue from ethyl acetate and ether there were obtained 4.0 g (84%) of 7-chloro-3-[3-(cyclopropyl-methoxy)- 1-propynyl]-4,5-dihydro-5 methyl6H-imidazo-[1,5-a][1,4]benzodiazepin-6-one of melting point 124-126°.

후처리

  1. additionwere added
  2. stirringThe reaction mixture was stirred at room temperature for 1 hour
  3. extractionThe mixture was extracted three times with methylene chloride
  4. washthe combined organic extracts were washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customBy crystallization of the residue from ethyl acetate

출처 및 근거

ORD 기록
ord-ca04ddd4043f4da1b3b0855929fe2b7f
출처 데이터셋
uspto-grants-1991_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05021411

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