Acetone → S 38093-2

HRID 1183803ノート

反応式

HRID 1183803 の反応式
[CH2:1]1[C@H:5]2[CH2:6][CH2:7][CH2:8][C@H:4]2[CH2:3][N:2]1[CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:21]=[CH:20][C:16]([C:17]([NH2:19])=[O:18])=[CH:15][CH:14]=1.CC(C)=O.[ClH:26]>O>[ClH:26].[CH2:1]1[C@H:5]2[CH2:6][CH2:7][CH2:8][C@H:4]2[CH2:3][N:2]1[CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:14]=[CH:15][C:16]([C:17]([NH2:19])=[O:18])=[CH:20][CH:21]=1

参加物

5

反応物 3

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 709411121403835-45-9

生成物 1

HCID 70945946S 38093-2収率 85%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

16.49 kg of 4-{3-[cis-hexahydrocyclopenta[c]pyrrol-2(1H)-yl]propoxy}benzamide, 16.36 kg of acetone, 6.76 kg of concentrated aqueous hydrochloric acid and 18.96 kg of water are introduced into a reactor. The mixture is stirred and heated at 50° C. for 1 hour. The mixture is then filtered in the hot state into a second reactor containing 57.67 kg of acetone and 1.65 kg of water. The mixture is then brought to reflux and 73.32 kg of acetone are added. Reflux is maintained for 10 minutes and then cooling to 0° C. is carried out. The product is filtered off and the solid obtained is washed with acetone. The product is obtained in the form of a powder in a yield of 85% and with a chemical purity greater than 99%.

後処理

  1. filtrationThe mixture is then filtered in the hot state into a second reactor
  2. additioncontaining 57.67 kg of acetone and 1.65 kg of water
  3. temperatureto reflux
  4. addition73.32 kg of acetone are added
  5. temperatureReflux
  6. temperatureis maintained for 10 minutes
  7. temperaturecooling to 0° C.
  8. filtrationThe product is filtered off
  9. customthe solid obtained
  10. washis washed with acetone
  11. customThe product is obtained in the form of a powder in a yield of 85% and with a chemical purity greater than 99%

出典と根拠

ORDレコード
ord-52b2484f01e34f7e9694cafedb88bb4c
出典データセット
uspto-grants-2014_03
特許番号
US08664408B2

反応ノート

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