Acetamidine monohydrochloride → HCID 178418769、化合物

HRID 2085081

反応式

HRID 2085081 の反応式
CO[C:3](=[O:18])[CH:4]([O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[O:16][CH3:17])[C:5]([O:7]C)=O.C[O-].[Na+].Cl.[C:23]([NH2:26])(=[NH:25])[CH3:24]>CO>[CH3:17][O:16][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[O:9][C:4]1[C:3]([OH:18])=[N:25][C:23]([CH3:24])=[N:26][C:5]=1[OH:7]

参加物

5

反応物 3

HCID 67170Acetamidine monohydrochlorideHCID 10942334Sodium MethoxideHCID 12967085Dimethyl 2-(2-methoxyphenoxy)malonate

生成物 1

HCID 178418769HCID 178418769、化合物収率 69.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 10 g of dimethyl-(o-methoxyphenoxy)malonate (Example 1b) in 80 ml dry methanol was cooled to 0° C. 6.71 g of sodium methylate was added portionenwise. To the suspension was added 2.84 g of acetamidine hydrochloride and the mixture was stirred overnight at room temperature. The solvent was removed under reduced pressure and the residue was suspended in 100 ml of diethyl ether. The solid was filtered off, washed with another portion of 100 ml of diethyl ether and dissolved in 50 ml of water. The pH was adjusted to 4 by adding 25 ml of glacial acetic acid. The white precipitate that formed was filtered off, washed with water and dried to yield 5.17 g of 5-(o-methoxyphenoxy)-4,6-dihydroxy-2-methyl-pyrimidine (or a tautomer) as a white powder.

後処理

  1. customThe solvent was removed under reduced pressure
  2. filtrationThe solid was filtered off
  3. washwashed with another portion of 100 ml of diethyl ether
  4. dissolutiondissolved in 50 ml of water
  5. additionby adding 25 ml of glacial acetic acid
  6. customThe white precipitate that formed
  7. filtrationwas filtered off
  8. washwashed with water
  9. customdried

出典と根拠

ORDレコード
ord-eab1ffd049c04bde8e2f3cc6f0bead7e
出典データセット
uspto-grants-2004_04
特許番号
US06720322B2

関連ノート

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