Tetrahydrofuran → HCID 86704992, 화합물

HRID 572188노트

반응식

HRID 572188 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16]2[C:21]([NH2:22])=[C:20]([CH3:23])[CH:19]=[CH:18][N:17]=2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:24]#[C:25]Br.C1COCC1.C(=O)([O-])O.[Na+]>O>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([N:15]2[C:16]3=[N:17][CH:18]=[CH:19][C:20]([CH3:23])=[C:21]3[N:22]=[C:25]2[NH2:24])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 10476Cyanogen BromideHCID 516892Sodium BicarbonateHCID 58577506N2-[4-(benzyloxy)phenyl]-4-methylpyridine-2,3-diamine

생성물 1

HCID 86704992HCID 86704992, 화합물수율 59.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of N2-[4-(benzyloxy)phenyl]-4-methylpyridine-2,3-diamine (8.70 g), cyanogen bromide (6.04 g), THF (80 ml) and water (20 ml) was stirred at room temperature for 24 hr. The reaction mixture was poured into saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was washed with ethyl acetate, treated with activated carbon, and recrystallized from methanol to give the title compound (5.60 g).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. washThe residue was washed with ethyl acetate
  6. additiontreated with activated carbon
  7. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-575689dd69734f7586fe74c67685dbd4
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029388B2

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