Hydrochloric Acid → HCID 178458062、化合物

HRID 2258177ノート

反応式

HRID 2258177 の反応式
[CH3:1]/[C:2](/[CH:8]=[N:9]/[N:10]=[C:11]([NH2:13])[NH2:12])=[N:3]\[N:4]=[C:5]([NH2:7])[NH2:6].Cl.C(O)(C)C>O>[CH3:1][C:2](=[N:3][NH:4][C:5](=[NH:6])[NH2:7])[CH:8]=[N:9][NH:10][C:11](=[NH:12])[NH2:13]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 5351154Mitoguazone

生成物 1

HCID 178458062HCID 178458062、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
30 °C

実験手順

A suspension of etude MGBG (460 g) in 920 g DI water was warmed to 40°-50° C. to give a clear pale yellow solution. The mixture was cooled to 30° C. and 920 mg conc. HCl was added. A pH of 0-1 was measured with litmus paper. Isopropanol (350 g, 446 mL) was added rapidly and the mixture stirred for 1 hour at 28°-32° C. The solutions were filtered to remove insoluble material. The filtrate was added to the reaction flask and acidified further with 0.5 g of conc. HCl The isopropanol (1.84 kg) was added over 10-15 minutes to the vigorously stirred solution. The mixture was cooled to 8°-12° C. and stirred for an additional hour. The solids were collected and the cake was rinsed with 2×200 mL isopropanol. After drying in a vacuum oven at 30°-40° C. for 24 hours, the recovery was about 90%. HPLC (ETI)=0.65%, nmr (dmsod6); IR (Kbr).

後処理

  1. temperaturewas warmed to 40°-50° C.
  2. customto give a clear pale yellow solution
  3. filtrationThe solutions were filtered
  4. customto remove insoluble material
  5. additionThe filtrate was added to the reaction flask
  6. additionwas added over 10-15 minutes to the vigorously stirred solution
  7. temperatureThe mixture was cooled to 8°-12° C.
  8. stirringstirred for an additional hour
  9. customThe solids were collected
  10. washthe cake was rinsed with 2×200 mL isopropanol
  11. customAfter drying in a vacuum oven at 30°-40° C. for 24 hours

出典と根拠

ORDレコード
ord-8404a4fcf5dc48fab0503be6c2eea922
出典データセット
uspto-grants-1997_08
特許番号
US05659083

反応ノート

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