Water → HCID 18183191, 화합물

HRID 430648

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HRID 430648 반응식
[CH:1]([C:3]1[CH2:9][C:8]2[CH:10]=[C:11]3[O:16][CH2:15][O:14][C:12]3=[CH:13][C:7]=2[C:6]([C:17]2[CH:22]=[CH:21][C:20]([N+:23]([O-:25])=[O:24])=[CH:19][CH:18]=2)=[N:5][N:4]=1)=[O:2].O.B([O-])=O.[Na+]>C1COCC1>[OH:2][CH2:1][C:3]1[CH2:9][C:8]2[CH:10]=[C:11]3[O:16][CH2:15][O:14][C:12]3=[CH:13][C:7]=2[C:6]([C:17]2[CH:22]=[CH:21][C:20]([N+:23]([O-:25])=[O:24])=[CH:19][CH:18]=2)=[N:5][N:4]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 145326Sodium metaborateHCID 108930778-formyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine

생성물 1

HCID 18183191HCID 18183191, 화합물수율 78.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
20 °C

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.

후처리

  1. stirringAfter 45 minutes of stirring
  2. filtrationit is filtered
  3. customthe crude product is precipitated from the filtrate with 130 ml of water
  4. custom2.35 g, which is recrystallized from a mixture of 6.3 ml of dimethylformamide and 1.3 ml of water
  5. customis obtained

출처 및 근거

ORD 기록
ord-999dd10ad7a0469f92ee27c353b9f1d3
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06323197B1

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