Hydrochloric Acid → 3-Carbamoyl-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide

HRID 22165

反応式

HRID 22165 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([O:11][C:12]2[CH:13]=[CH:14][CH:15]=[C:16]3[C:21]=2[C:19](=[O:20])[O:18][CH:17]3O)[N:4]=1.[C-:23]#[N:24].[K+].Cl.[OH2:27]>>[C:23]([CH:17]1[C:16]2[C:21](=[C:12]([O:11][C:5]3[N:4]=[C:3]([O:2][CH3:1])[CH:8]=[C:7]([O:9][CH3:10])[N:6]=3)[CH:13]=[CH:14][CH:15]=2)[C:19](=[O:20])[O:18]1)(=[O:27])[NH2:24]

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 9032Potassium CyanideHCID 199274177-[(4,6-Dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide

生成物 1

HCID 199274243-Carbamoyl-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide

実験手順

1.0 g of 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide (see Example 84) is introduced into a solution of 2.1 g of potassium cyanide in 15 ml of water and the whole is treated dropwise at from -7° to -3° C., with cooling, over a period of 10 minutes, with 10 ml of concentrated hydrochloric acid. It is subsequently stirred at room temperature for approximately 16 hours and the crystals which have separated are then filtered off. They are washed with water and recrystallised from acetone/n-hexane to yield 0.2 g of 3-carbamoyl-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide (see also Example 17).

後処理

  1. additionthe whole is treated dropwise at from -7° to -3° C.
  2. customthe crystals which have separated
  3. filtrationare then filtered off
  4. washThey are washed with water
  5. customrecrystallised from acetone/n-hexane

出典と根拠

ORDレコード
ord-5db9dc541d104704a857d69cebb76a01
出典データセット
uspto-grants-1995_06
特許番号
US05428002

関連ノート

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