Ammonia → HCID 385198、化合物

HRID 1421876ノート

反応式

HRID 1421876 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2([CH2:14][OH:15])[CH2:13][CH2:12][CH2:11]2)[CH:5]=[CH:4][N:3]=1.C([O-])(=O)C.[Na+].[Br:21]Br.N>C(O)(=O)C.O>[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2([CH2:14][OH:15])[CH2:13][CH2:12][CH2:11]2)[C:5]([Br:21])=[CH:4][N:3]=1

参加物

7

反応物 4

HCID 222AmmoniaHCID 24408BromineHCID 385194HCID 385194、化合物HCID 517045Sodium Acetate

生成物 1

HCID 385198HCID 385198、化合物収率 72.4%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 962Water溶媒

反応条件

温度
110 °C

実験手順

To 2-amino-4-[[(1-hydroxymethyl-1-cyclobutyl)methyl]amino]pyrimidine (0.21 g, 1.0 mmol) was added acetic acid (3 ml) and the mixture was heated to 110° C. Sodium acetate 3 hydrate (0.18 g) was added and bromine (60 μl) dissolved in acetic acid (0.5 ml) was dropwise added at 70° C. After cooling, water was added to the reaction mixture and the mixture was neutralized with aqueous ammonia under ice-cooling, extracted with ethyl acetate and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure and the residue was recrystallized from acetone to give colorless prism crystals (0.21 g, 72.4%), m.p. 156-158° C. (acetone).

後処理

  1. additionwas dropwise added at 70° C
  2. temperatureAfter cooling
  3. temperaturecooling
  4. extractionextracted with ethyl acetate
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled away under reduced pressure
  7. customthe residue was recrystallized from acetone

出典と根拠

ORDレコード
ord-e789c5d0393a40449349d26c8ae6d3d4
出典データセット
uspto-grants-2000_06
特許番号
US06080750

反応ノート

読み込み中…