Triethylamine → HCID 13338430、化合物

HRID 2417661ノート

反応式

HRID 2417661 の反応式
Cl.[CH3:2][O:3][C:4](=[O:8])[C@@H:5]([CH3:7])[NH2:6].C(N(CC)CC)C.Cl[C:17]1[C:18]2[N:26]([CH3:27])[N:25]=[C:24]([CH3:28])[C:19]=2[N:20]=[C:21]([CH3:23])[N:22]=1>CN(C)C=O>[CH3:27][N:26]1[C:18]2[C:17]([NH:6][C@H:5]([CH3:7])[C:4]([O:3][CH3:2])=[O:8])=[N:22][C:21]([CH3:23])=[N:20][C:19]=2[C:24]([CH3:28])=[N:25]1

参加物

5

反応物 3

HCID 8471Triethylamine2 回HCID 11182647Methyl D-alaninate hydrochlorideHCID 133384077-Chloro-1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidine

生成物 1

HCID 13338430HCID 13338430、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

D-alanine methyl ester hydrochloride (6 g, 0.043 mol) is dissolved in 30 ml of cold (5° C.) dimethylformamide and 7 ml (0.05 mol) of triethylamine is added dropwise. After stirring 15 minutes, 6 g of triethylamine hydrochloride is removed by filtering. To the filtrate is added 7 g (0.035 mol) of 7-chloro-1,3,5-trimethyl-1H-pyrazolo-[4,3-d]pyrimidine and another 6 ml of triethylamine. The mixture is stirred at 50°-55° C. for 60 hours and evaporated in vacuo. The residue is dissolved in 100 ml of methylene dichloride, washed with saturated sodium bicarbonate solution, dried over magnesium sulfate and evaporated in vacuo to give 7.6 g of slightly impure (R)-2-[1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidin-7-yl]aminopropionic acid, methyl ester, mp 68°-70° C. from ether as a dihydrate.

後処理

  1. additionis added dropwise
  2. custom6 g of triethylamine hydrochloride is removed
  3. filtrationby filtering
  4. stirringThe mixture is stirred at 50°-55° C. for 60 hours
  5. customevaporated in vacuo
  6. dissolutionThe residue is dissolved in 100 ml of methylene dichloride
  7. washwashed with saturated sodium bicarbonate solution
  8. dry with materialdried over magnesium sulfate
  9. customevaporated in vacuo

出典と根拠

ORDレコード
ord-000209ce74db4d59889b7b7f6f3a1b7e
出典データセット
uspto-grants-1984_09
特許番号
US04469868

反応ノート

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