1-(4-Methoxyphenyl)-piperazine, dihydrochloride → 3-{2-[4-(4-Methoxyphenyl)-1-piperazinyl]ethyl}-2-trifluoroacetylimino-6-trifluoromethoxybenzothiazoline hydrochloride

HRID 256826

反応式

HRID 256826 の反応式
[ClH:1].[CH3:2][O:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17]C3C4NC(=NC(=O)C(F)(F)F)SC=4C=C(OC(F)(F)F)C=3)[CH2:12][CH2:11]2)=[CH:6][CH:5]=1.CS(OCC[N:46]1[C:50]2[CH:51]=[CH:52][C:53]([O:55][C:56]([F:59])([F:58])[F:57])=[CH:54][C:49]=2[S:48][C:47]1=[N:60][C:61](=[O:66])[C:62]([F:65])([F:64])[F:63])(=O)=O.Cl.Cl.COC1C=CC(N2CCNCC2)=CC=1>C1(C)C=CC=CC=1>[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[CH:6][C:7]([N:10]2[CH2:11][CH2:12][N:13]([CH2:16][CH2:17][N:46]3[C:50]4[CH:51]=[CH:52][C:53]([O:55][C:56]([F:59])([F:57])[F:58])=[CH:54][C:49]=4[S:48][C:47]3=[N:60][C:61](=[O:66])[C:62]([F:63])([F:64])[F:65])[CH2:14][CH2:15]2)=[CH:8][CH:9]=1

参加物

5

反応物 3

HCID 27237001-(4-Methoxyphenyl)-piperazine, dihydrochlorideHCID 157348642-(2-Trifluoroacetylimino-6-trifluoromethoxy-3-benzothiazolinyl)ethyl methanesulphonateHCID 178491970HCID 178491970、化合物

生成物 1

HCID 197842683-{2-[4-(4-Methoxyphenyl)-1-piperazinyl]ethyl}-2-trifluoroacetylimino-6-trifluoromethoxybenzothiazoline hydrochloride

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

3-{2-[4-(4-Methoxyphenyl)-1-piperazinyl]ethyl-2-trifluoroacetylimino-6-trifluoromethoxybenzothiazoline hydrochloride may be prepared in the following manner: a mixture of 2-(2-trifluoroacetylimino-6-trifluoromethoxy-3-benzothiazolinyl)ethyl methanesulphonate (4.52 g), toluene (120 cc) and the base liberated from 4-(p-methoxyphenyl)piperazine dihydrochloride (10.56 g) is heated to reflux for 1 hour, cooled to +4° C. and then drained. The toluene filtrate is evaporated under reduced pressure and then treated with 1.2N aqueous hydrochloric acid solution (45 cc). The hydrochloride separates in amorphous form and then crystallizes on grinding with ethanol (50 cc). After draining, washing with ethanol (15 cc) and drying at 50° C. at 20 mmHg, 3-{2-[4-(4-methoxyphenyl)-1-piperazinyl]ethyl}-2-trifluoroacetylimino-6-trifluoromethoxybenzothiazoline hydrochloride (1.7 g) is obtained.

後処理

  1. temperatureis heated
  2. temperatureto reflux for 1 hour
  3. temperaturecooled to +4° C.
  4. customThe toluene filtrate is evaporated under reduced pressure
  5. additiontreated with 1.2N aqueous hydrochloric acid solution (45 cc)
  6. customcrystallizes
  7. customon grinding with ethanol (50 cc)
  8. washwashing with ethanol (15 cc)
  9. customdrying at 50° C. at 20 mmHg

出典と根拠

ORDレコード
ord-ee377dbe5f194db99304f6eff0dad590
出典データセット
uspto-grants-1993_11
特許番号
US05260297

関連ノート

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