Acetamidine monohydrochloride → HCID 178418769、化合物

HRID 1181222

反応式

HRID 1181222 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 dimethyl-(o-methoxyphenoxy)malonate (10 g) in dry methanol (80 ml) was cooled to 0° C. Sodium methylate (6.71 g) was added portionwise. To the suspension was added of acetamidine hydrochloride (2.84 g) and the mixture was stirred overnight at r.t. The solvent was removed under reduced pressure and the residue was suspended in diethyl ether (100 ml). The solid was filtered off, washed with another portion of diethyl ether (100 ml) and dissolved in water (50 ml). The pH was adjusted to 4 by adding glacial acetic acid (25 ml). The white precipitate that formed was filtered off, washed with water and dried to yield 5-(o-methoxyphenoxy)-4,6-dihydroxy-2-methyl-pyrimidine (5.17 g) (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 diethyl ether (100 ml)
  4. dissolutiondissolved in water (50 ml)
  5. additionby adding glacial acetic acid (25 ml)
  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-8a696d6f6c634383a218dad01bf1ed89
出典データセット
uspto-grants-2007_10
特許番号
US07285549B2

関連ノート

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