Stannous chloride dihydrate → N4-(3-Ethynylphenyl)quinazoline-4,6-diamine

HRID 1968641ノート

反応式

HRID 1968641 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([NH:9][C:10]2[C:19]3[C:14](=[CH:15][CH:16]=[C:17]([N+:20]([O-])=O)[CH:18]=3)[N:13]=[CH:12][N:11]=2)[CH:6]=[CH:7][CH:8]=1)#[CH:2].O.O.Cl[Sn]Cl.C([O-])(O)=O.[Na+]>C(OCC)(=O)C>[C:1]([C:3]1[CH:4]=[C:5]([NH:9][C:10]2[C:19]3[C:14](=[CH:15][CH:16]=[C:17]([NH2:20])[CH:18]=3)[N:13]=[CH:12][N:11]=2)[CH:6]=[CH:7][CH:8]=1)#[CH:2]

参加物

5

反応物 3

HCID 61436Stannous chloride dihydrateHCID 516892Sodium BicarbonateHCID 16045443N-(3-ethynylphenyl)-6-nitroquinazolin-4-amine

生成物 1

HCID 11492625N4-(3-Ethynylphenyl)quinazoline-4,6-diamine収率 89%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

N-(3-ethynylphenyl)-6-nitroquinazolin-4-amine (1.00 g, 3.45 mmol) and SnCl2.2H2O (3.10 g, 13.8 mmol) in ethyl acetate (35 mL) were refluxed for 2 h. After cooled to room temperature, the mixture was treated with 5% aqueous NaHCO3 to adjust its pH to 9-10 and then subjected to extraction with EtOAc. The combined organic layers were washed with saturated brine and H2O, dried, and concentrated under reduced pressure to give 0.79 g (89%) of N4-(3-ethynylphenyl)quinazoline-4,6-diamine as a yellow solid.

後処理

  1. extractionsubjected to extraction with EtOAc
  2. washThe combined organic layers were washed with saturated brine and H2O
  3. customdried
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-2aae24fbcb9f43b9a6d1da031fd01484
出典データセット
uspto-grants-2013_04
特許番号
US08426430B2

反応ノート

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