Dimethylformamide → HCID 18706853, 화합물

HRID 1421875노트

반응식

HRID 1421875 반응식
[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]=[C:4]([Cl:16])[N:3]=1.[Cl:17]N1C(=O)CCC1=O.CN(C)C=O>C(OCC)(=O)C>[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]([Cl:17])=[C:4]([Cl:16])[N:3]=1

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 31398ChlorosuccinimideHCID 385223HCID 385223, 화합물

생성물 1

HCID 18706853HCID 18706853, 화합물수율 54.2%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To 2-amino-6-chloro-4-[[(1-hydroxymethyl-1-cyclobutyl)methyl]amino]pyrimidine (0.24 g, 2.0 mmol) were added N-chlorosuccinimide (0.27 g, 2.0 mmol) and dimethylformamide (1.5 ml), and the mixture was stirred at room temperature for 2 days. Ethyl acetate was added and the mixture was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure and the residue was purified by silica gel column chromatography (chloroform:methanol=100:1) to give colorless prism crystals (0.3 g, 54.2%), m.p. 179-181° C. (acetone).

후처리

  1. washthe mixture was washed with water
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled away under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (chloroform:methanol=100:1)

출처 및 근거

ORD 기록
ord-225cb617e10e4cb4ba5b09eccd0edbd6
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06080750

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