Methane → Rilpivirine Hydrochloride

HRID 2280430ノート

反応式

HRID 2280430 の反応式
[CH3:1][C:2]1[CH:3]=[C:4](/[CH:25]=[CH:26]/[C:27]#[N:28])[CH:5]=[C:6]([CH3:24])[C:7]=1[NH:8][C:9]1[CH:10]=[CH:11][N:12]=[C:13]([NH:15][C:16]2[CH:17]=[CH:18][C:19]([C:22]#[N:23])=[CH:20][CH:21]=2)[N:14]=1.C.[ClH:30]>CO.C(C(C)=O)C.C(O)(C)C>[CH3:1][C:2]1[CH:3]=[C:4](/[CH:25]=[CH:26]/[C:27]#[N:28])[CH:5]=[C:6]([CH3:24])[C:7]=1[NH:8][C:9]1[CH:10]=[CH:11][N:12]=[C:13]([NH:15][C:16]2[CH:17]=[CH:18][C:19]([C:22]#[N:23])=[CH:20][CH:21]=2)[N:14]=1.[ClH:30]

参加物

7

反応物 3

HCID 297MethaneHCID 313Hydrochloric AcidHCID 6451164Rilpivirine

生成物 1

HCID 11711114Rilpivirine Hydrochloride

試薬・触媒・溶媒 3

HCID 887Methanol溶媒2 回HCID 3776Isopropanol溶媒HCID 6569Methyl Ethyl Ketone溶媒

反応条件

温度
62.5 °C

実験手順

Rilpivirine (20 gm; Chromatographic purity: 96.5%) was suspended in a mixture of methanol and methyl ethyl ketone (1:1, 2000 ml) and then heated to reflux for 1 hour to provide a clear solution. The solution was treated with charcoal and filtered through celite bed. The solvent was distilled off under reduced pressure to obtain a residual solid. To the residual solid was added methanol (200 ml) and then heated to 60 to 65° C. To the solution was added a solution of hydrochloric acid in isopropanol (200 ml) at 60 to 65° C. and stirred for 1 hour 30 minutes. The contents were cooled to room temperature and stirred for 30 minutes. The separated solid was filtered and then dried to provide 14 gm of rilpivirine hydrochloride.

後処理

  1. temperatureheated
  2. temperatureto reflux for 1 hour
  3. customto provide a clear solution
  4. filtrationfiltered through celite bed
  5. distillationThe solvent was distilled off under reduced pressure
  6. customto obtain a residual solid
  7. temperatureThe contents were cooled to room temperature
  8. stirringstirred for 30 minutes
  9. filtrationThe separated solid was filtered
  10. customdried

出典と根拠

ORDレコード
ord-83b3be3bfaaa40a09965ecec7c8f2a08
出典データセット
uspto-grants-2015_09
特許番号
US09139535B2

反応ノート

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