Tetrahydrofuran → HCID 86704992、化合物

HRID 572188ノート

反応式

HRID 572188 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 86704992HCID 86704992、化合物収率 59.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-575689dd69734f7586fe74c67685dbd4
出典データセット
uspto-grants-2015_05
特許番号
US09029388B2

反応ノート

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