Phosphorus oxychloride → 4-Chloro-7-ethoxy-6-methoxyquinazoline

HRID 1917634노트

반응식

HRID 1917634 반응식
[CH2:1]([O:3][C:4]1[CH:13]=[C:12]2[C:7]([C:8](=O)[NH:9][CH:10]=[N:11]2)=[CH:6][C:5]=1[O:15][CH3:16])[CH3:2].O=P(Cl)(Cl)[Cl:19]>C1(C)C=CC=CC=1>[Cl:19][C:8]1[C:7]2[C:12](=[CH:13][C:4]([O:3][CH2:1][CH3:2])=[C:5]([O:15][CH3:16])[CH:6]=2)[N:11]=[CH:10][N:9]=1

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 1355332107-ethoxy-6-methoxyquinazolin-4(3H)-one

생성물 1

HCID 117705294-Chloro-7-ethoxy-6-methoxyquinazoline수율 96%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 7-ethoxy-6-methoxyquinazolin-4(3H)-one (1.20 g, 5.45 mmol) and POCl3 (3 mL), in toluene (10 mL) was heated at 125° C. for 5 hours. It was concentrated under reduced pressure to dryness. To it was added CH2Cl2 and it was washed with saturated NaHCO3. The organic layer was dried over MgSO4 and concentrated to give 4-chloro-7-ethoxy-6-methoxyquinazoline as solid (1.254 g, 96%). 1H NMR (300 MHz, CDCl3) δ 8.91 (s, 1H), 7.52 (s, 1H), 7.42 (s, 1H), 4.34 (q, 2H), 4.08 (s, 3H), 1.59 (t, 3H).

후처리

  1. concentrationIt was concentrated under reduced pressure to dryness
  2. additionTo it was added CH2Cl2 and it
  3. washwas washed with saturated NaHCO3
  4. dry with materialThe organic layer was dried over MgSO4
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1f5c405e738a4921af3eaba2101ece8b
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618289B2

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