Chloroacetyl chloride → HCID 68283152、化合物

HRID 624029ノート

反応式

HRID 624029 の反応式
[CH3:1][O:2][C:3]1[C:8]([O:9][CH3:10])=[CH:7][N:6]=[C:5]([NH2:11])[N:4]=1.CCN(C(C)C)C(C)C.[Cl:21][CH2:22][C:23](Cl)=[O:24]>C(Cl)Cl>[Cl:21][CH2:22][C:23]([NH:11][C:5]1[N:4]=[C:3]([O:2][CH3:1])[C:8]([O:9][CH3:10])=[CH:7][N:6]=1)=[O:24]

参加物

5

反応物 3

HCID 6577Chloroacetyl chlorideHCID 81531DiisopropylethylamineHCID 129881044,5-Dimethoxypyrimidin-2-amine

生成物 1

HCID 68283152HCID 68283152、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4,5-dimethoxypyrimidin-2-amine (350 mg, 2.26 mmol) in DCM (3.5 mL), DIPEA (1.2 mL, 7.0 mmol) was added, followed by chloracetylchloride (0.30 mL, 3.72 mmol). The resulting dark brown reaction mixture was stirred at rt for 1 h, then quenched with water and diluted with DCM. The org. layer was separated and the aq. layer extracted with DCM (1×). The combined org. layers were washed with brine, dried (MgSO4), filtered and the solvent removed under reduced pressure to obtain 2-chloro-N-(4,5-dimethoxypyrimidin-2-yl)acetamide as a brown oil which was used in the next step without further purification. LC-MS conditions B: tR=0.38 min, [M+H]+=232.07.

後処理

  1. customquenched with water
  2. additiondiluted with DCM
  3. customlayer was separated
  4. extractionthe aq. layer extracted with DCM (1×)
  5. washlayers were washed with brine
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-d05eb4b1be0a4428a98ffc64274d35bb
出典データセット
uspto-grants-2016_04
特許番号
US09303023B2

反応ノート

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