Phosgene → 2-Chloro-6-iodo-3-propyl-quinazolin-4-one

HRID 1276610ノート

反応式

HRID 1276610 の反応式
[I:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=S)[N:6]([CH2:13][CH2:14][CH3:15])[C:5]2=[O:16].C(Cl)([Cl:19])=O>C1(C)C(C)=CC=CC=1>[Cl:19][C:7]1[N:6]([CH2:13][CH2:14][CH3:15])[C:5](=[O:16])[C:4]2[C:9](=[CH:10][CH:11]=[C:2]([I:1])[CH:3]=2)[N:8]=1

参加物

4

反応物 2

HCID 6371PhosgeneHCID 108933556-iodo-3-propyl-2-thioxo-2,3-dihydroquinazolin-4(1H)-one

生成物 1

HCID 108610142-Chloro-6-iodo-3-propyl-quinazolin-4-one

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
87.5 °C

実験手順

2,3-Dihydro-6-iodo-3-propyl-2-thioxo4(1H)-quinazolinone (50 g, 0.144 mol) was slurried in xylene (283 g) and heated to 85-90° C. Phosgene (12.0 mL, 0.159 mol) was added. Heating was continued until the thioquinazolinedione was consumed by thin layer chromatography analysis (340 minutes). The excess phosgene was removed by codistillation with xylene at atmospheric pressure. The distillation was ceased when the distillate weight reached 37.9 g. The solution was cooled to room temperature and used directly in Step 3.

後処理

  1. temperatureHeating
  2. customwas consumed by thin layer chromatography analysis (340 minutes)
  3. customThe excess phosgene was removed by codistillation with xylene at atmospheric pressure
  4. distillationThe distillation
  5. temperatureThe solution was cooled to room temperature

出典と根拠

ORDレコード
ord-6567a2b7ac424cdab5bdaf8768cd0397
出典データセット
uspto-grants-2000_12
特許番号
US06166208

反応ノート

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