1,3-Dichloro-2-isocyanatobenzene → HCID 57710265, 화합물

HRID 1038697노트

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HRID 1038697 반응식
[CH3:1][N:2]([CH3:18])[C:3]1[CH:4]=[C:5]([NH:9][C:10]2[CH:15]=[C:14]([NH:16][CH3:17])[N:13]=[CH:12][N:11]=2)[CH:6]=[CH:7][CH:8]=1.[Cl:19][C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[C:21]=1[N:27]=[C:28]=[O:29]>CN(C)C=O>[Cl:19][C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[C:21]=1[NH:27][C:28](=[O:29])[N:16]([C:14]1[CH:15]=[C:10]([NH:9][C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([N:2]([CH3:1])[CH3:18])[CH:4]=2)[N:11]=[CH:12][N:13]=1)[CH3:17]

참가 물질

4

반응물 2

HCID 6045371,3-Dichloro-2-isocyanatobenzene2회HCID 66670065HCID 66670065, 화합물

생성물 1

HCID 57710265HCID 57710265, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
90 °C

실험 절차

A mixture of N-(3-dimethylamino-phenyl)-N′-methyl-pyrimidine-4,6-diamine (243.3 mg, 1 mmol), 2,6-dichlorophenyl isocyanate (188 mg, 1 mmol) in dry dimethylformamide (2.5 mL) is shaken for 14 h at 90° C. Two additional portions (188 mg, 1 mmol each) of 2,6-dichlorophenyl isocyanate are added after 14 h and 26 h. After 38 h the reaction mixture is evaporated in vacuo and the residue is distributed between ethyl acetate and half-saturated K2CO3 solution. The organic layer is dried over Na2SO4, evaporated, and the residue purified by flash chromatography (hexane/ethyl acetate). The combined pure fractions are evaporated, the residue triturated with CH2Cl2 and the solid filtered off and dried in vacuo to afford the title compound.

후처리

  1. customAfter 38 h the reaction mixture is evaporated in vacuo
  2. dry with materialThe organic layer is dried over Na2SO4
  3. customevaporated
  4. customthe residue purified by flash chromatography (hexane/ethyl acetate)
  5. customThe combined pure fractions are evaporated
  6. customthe residue triturated with CH2Cl2
  7. filtrationthe solid filtered off
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-a051174cb3594565b1c1c74ff41a554b
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552002B2

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