Chloroacetyl chloride → HCID 68283152, 화합물

HRID 624029노트

반응식

HRID 624029 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 68283152HCID 68283152, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d05eb4b1be0a4428a98ffc64274d35bb
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09303023B2

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