Hydrochloric Acid → HCID 131720060、化合物

HRID 362737ノート

反応式

HRID 362737 の反応式
[F:1][C:2]1[CH:3]=[C:4]([C:9]2([CH2:28][CH2:29]OS(C)(=O)=O)[O:14][CH2:13][CH2:12][N:11]([C:15](=[O:27])[CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([O:23][CH:24]([CH3:26])[CH3:25])[CH:18]=3)[CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8].[N:35]1([CH:41]2[CH2:46][CH2:45][NH:44][CH2:43][CH2:42]2)[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]1.O.[ClH:48]>CN(C=O)C.CCOCC>[OH2:14].[ClH:48].[ClH:48].[F:1][C:2]1[CH:3]=[C:4]([C:9]2([CH2:28][CH2:29][N:44]3[CH2:45][CH2:46][CH:41]([N:35]4[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]4)[CH2:42][CH2:43]3)[O:14][CH2:13][CH2:12][N:11]([C:15](=[O:27])[CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([O:23][CH:24]([CH3:26])[CH3:25])[CH:18]=3)[CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8].[F:1][C:2]1[CH:3]=[C:4]([C:9]2([CH2:28][CH2:29][N:44]3[CH2:45][CH2:46][CH:41]([N:35]4[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]4)[CH2:42][CH2:43]3)[O:14][CH2:13][CH2:12][N:11]([C:15](=[O:27])[CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([O:23][CH:24]([CH3:26])[CH3:25])[CH:18]=3)[CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8].[ClH:48].[ClH:48]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 786071,4'-BipiperidineHCID 21200564HCID 21200564、化合物

生成物 1

HCID 131720060HCID 131720060、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

A mixture of 1.3 g of the compound obtained in step C of EXAMPLE 71 and 1.1 g of 4-(piperid-1-yl)-piperidine in 4 ml of DMF is heated at 70° C. for 4 hours. After cooling to RT, the reaction mixture is poured into iced water and extracted with AcOEt, the organic phase is washed with 1N NaOH solution and with saturated NaCl solution and dried over Na2SO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica H using DCM and then a DCM/MeOH mixture (90/10; v/v) as the eluent. The product obtained is taken up with a saturated solution of hydrochloric acid in ether and the precipitate formed is wrung to give 0.49 g of the expected product. M.p.=270° C. (dec.).

後処理

  1. temperatureAfter cooling to RT
  2. extractionextracted with AcOEt
  3. washthe organic phase is washed with 1N NaOH solution and with saturated NaCl solution
  4. dry with materialdried over Na2SO4
  5. customthe solvent is evaporated off under vacuum
  6. customThe residue is chromatographed on silica H
  7. customThe product obtained
  8. customthe precipitate formed

出典と根拠

ORDレコード
ord-c0657193a8f840abac4629d2c5c190d9
出典データセット
uspto-grants-1999_02
特許番号
US05869663

反応ノート

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