반응 #517830

반응 방정식

8-formyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine

water

sodium boranate

→

title compound

수율 78.4%

8-Hydroxymethyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine

수율 78.4%

용매

THF

반응 조건

후처리

1. 1
   workup.STIRRINGAfter 45 minutes of stirring
2. 2
   여과it is filtered
3. 3
   기타the crude product is precipitated from the filtrate with 130 ml of water
4. 4
   기타2.35 g, which is recrystallized from a mixture of 6.3 ml of dimethylformamide and 1.3 ml of water
5. 5
   기타is obtained

실험 절차

2.5 g (7.41 mmol) of 8-formyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine (I, stage A) is suspended in THF:water=1:1 and mixed with 0.14 g (3.7 mmol) of sodium boranate while being stirred and cooled to 20° C. After 45 minutes of stirring, it is filtered and the crude product is precipitated from the filtrate with 130 ml of water. 2.35 g, which is recrystallized from a mixture of 6.3 ml of dimethylformamide and 1.3 ml of water, is obtained. 1.97 g (78%) of the title compound with a melting point of 175° C. (decomposition) is obtained.

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