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Formamidine acetate → HCID 178487763, 화합물

HRID 1811049
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HRID 1811049 반응식
[NH2:1][C:2]1[CH:10]=[C:9]([O:11][CH3:12])[CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5].C(O)(=O)C.[CH:17](N)=[NH:18]>COCCO>[CH3:12][O:11][C:9]1[CH:10]=[C:2]2[C:3]([C:4]([OH:5])=[N:18][CH:17]=[N:1]2)=[CH:7][CH:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 160693Formamidine acetateHCID 3510102-Amino-4-methoxybenzoic acid

생성물 1

HCID 178487763HCID 178487763, 화합물수율 90%

시약·촉매·용매 1

HCID 80192-Methoxyethanol용매

반응 조건

온도
130 °C

실험 절차

Step 1 A mixture of 2-amino-4-methoxybenzoic acid (0.5 g, 2.99 mmol) and formamidine acetate (0.623 g, 5.98 mmol) in 2-methoxyethanol (4 mL) was heated at 130° C. After 15.25 h, the mixture was cooled to rt. The resulting precipitate was collected by filtration, washed with methanol and dried to provide 7-methoxyquinazolin-4-ol as a tan solid (473 mg, 90%). 1H NMR (400 MHz, DMSO-d6) δ 12.08 (1 H, br. s.), 8.06 (1 H, s), 8.03 (1 H, d, J=9.5 Hz), 7.03-7.14 (2 H, m), 3.90 (3 H, s).

후처리

  1. temperaturethe mixture was cooled to rt
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with methanol
  4. customdried

출처 및 근거

ORD 기록
ord-dbb7e3abeda4448e845102690cab76c6
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08362065B2

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