Acetic Anhydride → 4-(1-Acetyl-4-piperidinyl)-2-aminoquinazoline

HRID 617178ノート

反応式

HRID 617178 の反応式
[NH2:1][C:2]1[N:11]=[C:10]([CH:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.C(N(CC)CC)C.[C:25](OC(=O)C)(=[O:27])[CH3:26]>CN(C)C=O>[C:25]([N:15]1[CH2:16][CH2:17][CH:12]([C:10]2[C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[N:3]=[C:2]([NH2:1])[N:11]=2)[CH2:13][CH2:14]1)(=[O:27])[CH3:26]

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 154287752-Amino-4-(4-piperidinyl)quinazoline

生成物 1

HCID 154287764-(1-Acetyl-4-piperidinyl)-2-aminoquinazoline収率 76.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To an ice-cold solution of 2-amino-4-(4-piperidyl)quinazoline (500 mg, 2.19 mmol) and triethylamine (233 mg, 2.3 mmol) in N,N-dimethylformamide (10 ml) was added dropwise acetic anhydride (0.22 ml, 2.30 mmol) under a nitrogen atmosphere. The reaction mixture was stirred for about 3 hours and was evaporated. The residue was partitioned between dichloromethane and saturated sodium hydrogencarbonate aqueous solution. The organic layer was washed with water and then dried over sodium sulfate and evaporated in vacuo. The residue was crystallized from ethanol. Recrystallization from methanol gave the titled compound(452 mg).

後処理

  1. customwas evaporated
  2. customThe residue was partitioned between dichloromethane and saturated sodium hydrogencarbonate aqueous solution
  3. washThe organic layer was washed with water
  4. dry with materialdried over sodium sulfate
  5. customevaporated in vacuo
  6. customThe residue was crystallized from ethanol
  7. customRecrystallization from methanol

出典と根拠

ORDレコード
ord-260fcdb2392148ba881ea8ed6c2255f6
出典データセット
uspto-grants-1999_09
特許番号
US05948786

反応ノート

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