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Hydrochloric Acid → HCID 14010769, 화합물

HRID 255674
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HRID 255674 반응식
C([O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:20]([CH:21]=[O:22])=[CH:19][C:18](=[O:23])[C:13]([C:14]([O:16]C)=[O:15])=[CH:12]2)=[C:7]([CH3:24])[CH:6]=1)(=O)C.Cl.C(=O)([O-])O.[Na+].[Cl-].[Na+]>C(#N)C>[CH:21]([C:20]1[N:11]([C:8]2[CH:9]=[CH:10][C:5]([OH:4])=[CH:6][C:7]=2[CH3:24])[CH:12]=[C:13]([C:18](=[O:23])[CH:19]=1)[C:14]([OH:16])=[O:15])=[O:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 516892Sodium BicarbonateHCID 14010755HCID 14010755, 화합물

생성물 1

HCID 14010769HCID 14010769, 화합물수율 76.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To 0.95 g of methyl 1-(4-acetoxy-2-methylphenyl)-6-formyl-4-oxo-1,4-dihydronicotinate was added 5 ml of 6N hydrochloric acid, and they were reacted at 100° C. for one hour. The reaction mixture was cooled to room temperature, and adjusted to a pH of 7.5 with a saturated aqueous sodium hydrogencarbonate solution. Then, 100 ml of acetonitrile was added, and the aqueous layer was saturated with sodium chloride. The organic layer was separated, washed with a saturated aqueous solution of sodium chloride and then dried with anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure to obtain 0.6 g of 6-formyl-1-(4-hydroxy-2-methylphenyl)-4-oxo-1,4-dihydronicotinic acid having a melting point of 230°-250° C.

후처리

  1. customwere reacted at 100° C. for one hour
  2. customThe organic layer was separated
  3. washwashed with a saturated aqueous solution of sodium chloride
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe solvent was removed by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-985f4584075d45a4bf2606e943c67c5f
출처 데이터셋
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04698352

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