HCID 18374925、化合物 → HCID 9877992、化合物

HRID 2300064ノート

反応式

HRID 2300064 の反応式
[CH3:1][N:2]1[C:7]2[N:8]=[C:9](S(C)(=O)=O)[N:10]=[CH:11][C:6]=2[CH:5]=[CH:4][C:3]1=[O:16]>C(N)CCC>[CH2:3]([NH:2][C:9]1[N:10]=[CH:11][C:6]2[CH:5]=[CH:4][C:3](=[O:16])[N:2]([CH3:1])[C:7]=2[N:8]=1)[CH2:4][CH2:5][CH3:6]

参加物

3

反応物 1

HCID 18374925HCID 18374925、化合物

生成物 1

HCID 9877992HCID 9877992、化合物収率 159.8%

試薬・触媒・溶媒 1

HCID 8007Butylamine溶媒

実験手順

A solution of 8-methyl-2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one (200 mg, 0.83 mmol) in 2 mL of n-butylamine was stirred at room temperature for 10 minutes. The reaction mixture was partitioned between ethyl acetate and water, and the organic layer was washed with saturated sodium bicarbonate and brine, dried over magnesium sulfate, and concentrated in vacuo. A 4:1 mixture of hexane:ethyl acetate was added to the residue and the resultant solid collected by filtration to give 154 mg (79%) of 2-butylamino-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one, mp 146-147° C.

後処理

  1. customThe reaction mixture was partitioned between ethyl acetate and water
  2. washthe organic layer was washed with saturated sodium bicarbonate and brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. additionA 4:1 mixture of hexane
  6. additionethyl acetate was added to the residue
  7. filtrationthe resultant solid collected by filtration

出典と根拠

ORDレコード
ord-1af32eed8c99406daa91afaab1806f40
出典データセット
uspto-grants-2002_12
特許番号
US06498163B1

反応ノート

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