Sodium Azide → 6-Azido-4-[2-(6-fluoro-pyridin-2-yl)-imidazol-1-ylmethyl]-5-propyl-pyrimidine

HRID 916638노트

반응식

HRID 916638 반응식
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([CH2:8][N:9]2[CH:13]=[CH:12][N:11]=[C:10]2[C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[N:15]=2)[C:3]=1[CH2:21][CH2:22][CH3:23].[N-:24]=[N+:25]=[N-:26].[Na+]>CN(C=O)C>[N:24]([C:2]1[N:7]=[CH:6][N:5]=[C:4]([CH2:8][N:9]2[CH:13]=[CH:12][N:11]=[C:10]2[C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[N:15]=2)[C:3]=1[CH2:21][CH2:22][CH3:23])=[N+:25]=[N-:26]

참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 223131636-Chloro-4-[2-(6-fluoro-pyridin-2-yl)-imidazol-1-ylmethyl]-5-propyl-pyrimidine

생성물 1

HCID 223131686-Azido-4-[2-(6-fluoro-pyridin-2-yl)-imidazol-1-ylmethyl]-5-propyl-pyrimidine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 103 (2.25 mmol) and NaN3 (731 mg, 11.25 mmol) in DMF (15 ml) is heated at 70° C. in a sealed tube overnight. The solvent is removed in vacuo and water (10 ml) and EtOAc (10 ml) are added to the residue. The layers are separated and the aqueous layer is extracted with EtOAc (2×10 ml). The combined extracts are washed with brine (15 ml) and dried with Na2SO4. The solvent is removed in vacuo and the resulting yellow oil (104) is used in the next step without further purification.

후처리

  1. customThe solvent is removed in vacuo and water (10 ml) and EtOAc (10 ml)
  2. additionare added to the residue
  3. customThe layers are separated
  4. extractionthe aqueous layer is extracted with EtOAc (2×10 ml)
  5. washThe combined extracts are washed with brine (15 ml)
  6. dry with materialdried with Na2SO4
  7. customThe solvent is removed in vacuo
  8. customthe resulting yellow oil (104) is used in the next step without further purification

출처 및 근거

ORD 기록
ord-c180fc79222d413f9fdc97e62223fd66
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07271170B2

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