Hydrochloric Acid → HCID 22312924, 화합물

HRID 351566노트

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HRID 351566 반응식
[Cl:1][C:2]1[CH:23]=[CH:22][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([N:14]3[C:19](=[O:20])[NH:18][C:17](=[O:21])[CH:16]=[N:15]3)=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.[OH-].[Na+].[BH4-].[Na+].Cl>O.C(O)C>[Cl:1][C:2]1[CH:23]=[CH:22][C:5]([CH:6]([OH:7])[C:8]2[CH:9]=[CH:10][C:11]([N:14]3[C:19](=[O:20])[NH:18][C:17](=[O:21])[CH:16]=[N:15]3)=[CH:12][CH:13]=2)=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2회HCID 4311764Sodium borohydrideHCID 12846566HCID 12846566, 화합물

생성물 1

HCID 22312924HCID 22312924, 화합물수율 35.2%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

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온도
10 °C

실험 절차

A mixture of 2-[4-(4-chlorobenzoyl)phenyl]-1,2,4-triazine-3,5-(2H,4H)-dione (0.05 mol), ethanol (150 ml), water (150 ml) and NaOH (50%; 10 ml) was stirred at 10° C. A mixture of NaBH4 (0.05 mol), water (50 ml) and NaOH (50%; 2 ml) was added dropwise during 15 minutes. After stirring for 3 hours, 300 ml ice was added. The mixture was acidified with concentrated HCl. The product was extracted with CHCl3, yielding 5.8 g of 2-[4-[(4-chlorophenyl)hydroxymethyl]phenyl]-1,2,4-triazine-3,5-(2H,4H)-dione (intern. 31). The organic layer was dried, filtered and evaporated. The residue was crystallized with 2-propanol. The product was filtered off, washed with 2,2′-oxybispropane and dried, yielding a second fraction of 5.5 g of intermediate 31.

후처리

  1. additionwas added dropwise during 15 minutes
  2. stirringAfter stirring for 3 hours
  3. extractionThe product was extracted with CHCl3

출처 및 근거

ORD 기록
ord-b938c8a79c50452da4d793d7b4a84056
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06743792B2

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