HCID 10861014、化合物 → Proquinazid

HRID 1276611

反応式

HRID 1276611 の反応式
[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]

参加物

4

反応物 2

HCID 10861014HCID 10861014、化合物HCID 236693631-Propanol, sodium salt (1:1)

生成物 1

HCID 11057771Proquinazid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
1 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-25846c65a19b4fee91b602fdfb7cffc6
出典データセット
uspto-grants-2000_12
特許番号
US06166208

関連ノート

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