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Acetic Acid → 2-Ethoxymethyl-6-methyl-4(3H)-pteridinone

HRID 1681044
ノート
印刷プレビュー

反応式

HRID 1681044 の反応式
N[C:2]1[C:11]2[C:6](=[N:7][CH:8]=[C:9]([CH3:12])[N:10]=2)[N:5]=[C:4]([CH2:13][O:14][CH2:15][CH3:16])[N:3]=1.C(O)(=[O:19])C>[OH-].[Na+]>[CH2:15]([O:14][CH2:13][C:4]1[NH:3][C:2](=[O:19])[C:11]2[C:6](=[N:7][CH:8]=[C:9]([CH3:12])[N:10]=2)[N:5]=1)[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 176Acetic AcidHCID 107275934-Amino-2-ethoxymethyl-6-methylpteridine

生成物 1

HCID 1355283202-Ethoxymethyl-6-methyl-4(3H)-pteridinone

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒2 回

実験手順

A suspension of 7.4 g (0.0338 mole) of 4-amino-2-ethoxymethyl-6-methylpteridine in 148 ml of 5% aqueous sodium hydroxide is brought slowly to 85° C. and maintained at this temperature for 2 hours. A further 592 ml of 5% aqueous sodium hydroxide are then added and heating is contained at 85° C. for 1 hour. After cooling, the solution obtained is acidified with acetic acid to pH 5.5, and is then extracted with dichloromethane. The organic extracts are dried over sodium sulphate and concentrated to dryness under reduced pressure. The solid residue is recrystallized from acetone in the presence of Norit. Yld: 4.9 g (66%), m.p. 181°-183° C.

後処理

  1. customis brought slowly to 85° C.
  2. temperaturemaintained at this temperature for 2 hours
  3. temperatureheating
  4. temperatureAfter cooling
  5. customthe solution obtained
  6. extractionis then extracted with dichloromethane
  7. dry with materialThe organic extracts are dried over sodium sulphate
  8. concentrationconcentrated to dryness under reduced pressure
  9. customThe solid residue is recrystallized from acetone in the presence of Norit

出典と根拠

ORDレコード
ord-b7b47836e841466190a6e13be7a63cc0
出典データセット
uspto-grants-1992_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05167949

反応ノート

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