Dimethylamine → HCID 22899422、化合物

HRID 409506

反応式

HRID 409506 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([C:9](Cl)=[O:10])=[CH:4][N:3]=1.[NH:12]([CH3:14])[CH3:13].CCN(CC)CC.O>C(Cl)Cl>[CH3:13][N:12]([CH3:14])[C:9]([C:5]1[C:6]([Cl:8])=[N:7][C:2]([Cl:1])=[N:3][CH:4]=1)=[O:10]

参加物

6

反応物 4

HCID 674DimethylamineHCID 962WaterHCID 8471TriethylamineHCID 137841122,4-Dichloropyrimidine-5-carbonyl chloride

生成物 1

HCID 22899422HCID 22899422、化合物収率 158.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2,4-dichloro-pyrimidine-5-carbonyl chloride (197.7 mg, 0.94 mmol) in CH2Cl2 (9.4 mL) at RT is added Me2NH (2.0 M THF solution, 390 μL, 0.78 mmol) and Et3N (108.6 μL, 0.78 mmol) at 0° C. The reaction mixture is stirred overnight at RT. After adding water, the mixture is extracted with CH2Cl2. The organic layer is dried and concentration under reduce pressure give 2,4-dichloro-pyrimidine-5-carboxylic acid dimethylamide (272.5 mg, quant). ESI-MS m/z: 221 [M+1]+, Retention time 1.94 min (condition B).

後処理

  1. extractionthe mixture is extracted with CH2Cl2
  2. customThe organic layer is dried
  3. concentrationconcentration

出典と根拠

ORDレコード
ord-856aba5aff5341e091ab4f4ba329994d
出典データセット
uspto-grants-2014_06
特許番号
US08759365B2

関連ノート

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