HCID 10861014, 화합물 → Proquinazid

HRID 1276611

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HRID 1276611 반응식
[O-:1][CH2:2][CH2:3][CH3:4].[Na+].Cl[C:7]1[N:16]([CH2:17][CH2:18][CH3:19])[C:15](=[O:20])[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([I:21])[CH:13]=2)[N:8]=1>O>[I:21][C:12]1[CH:13]=[C:14]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([O:1][CH2:2][CH2:3][CH3:4])[N:16]([CH2:17][CH2:18][CH3:19])[C:15]2=[O:20]

참가 물질

4

반응물 2

HCID 10861014HCID 10861014, 화합물HCID 236693631-Propanol, sodium salt (1:1)

생성물 1

HCID 11057771Proquinazid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
1 °C

실험 절차

A portion of the sodium propoxide solution prepared above (87 g) was cooled to 1° C. and treated dropwise with the solution of 2-chloro-6-iodo-3-n-propyl-4(3H)-quinazolinone prepared in Step 2B above. The temperature was maintained at or below 0° C. and the addition took 2.5 h. After stirring at 0° C. for an additional 1.5 h, the reaction mixture was poured into 250 mL water. The phases were separated and the organic phase was washed two times each with 250 mL water. The organic phase was then evaporated under reduced pressure to give 53.4 g of a light yellow oil which solidified upon standing to a white solid. mp 60-62° C.; 1H NMR (CDCl3): δ8.49 (d,1H), 7.87 (dd,1H), 7.19 (d,1H), 4.43 (t,2H), 4.05 (m,2H), 1.85 (m,2H), 1.70 (m,2H), 1.05 (t,3H), 0.96 (t,3H).

후처리

  1. temperatureThe temperature was maintained at or below 0° C.
  2. additionthe addition
  3. customThe phases were separated
  4. washthe organic phase was washed two times each with 250 mL water
  5. customThe organic phase was then evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-25846c65a19b4fee91b602fdfb7cffc6
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06166208

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