Ammonium Chloride → HCID 178487492, 화합물

HRID 392581

반응식

HRID 392581 반응식
[NH:1]1[CH:5]=[C:4]([C:6]([C:8]2[CH:17]=[CH:16][C:15]3[C:10](=[CH:11][CH:12]=[C:13]([O:18][CH3:19])[CH:14]=3)[CH:9]=2)=[O:7])[N:3]=[CH:2]1.[CH:20]([Mg]Cl)([CH3:22])[CH3:21].[Cl-].[NH4+]>C1COCC1.O>[NH:1]1[CH:5]=[C:4]([C:6]([C:8]2[CH:17]=[CH:16][C:15]3[C:10](=[CH:11][CH:12]=[C:13]([O:18][CH3:19])[CH:14]=3)[CH:9]=2)([OH:7])[CH:20]([CH3:22])[CH3:21])[N:3]=[CH:2]1

참가 물질

6

반응물 3

HCID 25517Ammonium ChlorideHCID 178418918HCID 178418918, 화합물HCID 178487490HCID 178487490, 화합물

생성물 1

HCID 178487492HCID 178487492, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

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온도
-10 °C

실험 절차

(1H-Imidazol-4-yl)-(6-methoxynaphthalen-2-yl)ketone (6.50 g) was dissolved in THF (120 ml) and the mixture was cooled to −10° C. A solution (2.0 M; 38.7 ml) of isopropyl magnesium chloride in THF was slowly added dropwise and the mixture was stirred for 30 min. To the reaction mixture was added saturated aqueous solution of ammonium chloride and the mixture was diluted with water and extracted with ethyl acetate. The extract was washed with saturated brine, and after drying, concentrated. The obtained residue was purified by silica gel column chromatography (eluate, chloroform:methanol=20:1→10:1) and recrystallized from ethyl acetate to give the title compound (5.04 g) as a colorless crystalline powder.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. customafter drying
  4. concentrationconcentrated
  5. customThe obtained residue was purified by silica gel column chromatography (eluate, chloroform:methanol=20:1→10:1)
  6. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-26c6fc93a0014f97bc37693d9637e63e
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06800778B1

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