Sodium Hydroxide → HCID 20283107、化合物

HRID 463322ノート

反応式

HRID 463322 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2([CH2:19][CH2:20][CH2:21][N:22]([CH2:24][C:25]([N:27]3[CH2:32][CH2:31][CH:30]([O:33][C:34]4[CH:39]=[CH:38][C:37]([Cl:40])=[CH:36][CH:35]=4)[CH2:29][CH2:28]3)=O)[CH3:23])[O:18][CH2:17][CH2:16][O:15]2)=[CH:10][CH:9]=1.C([O-])(=O)C([O-])=O.[OH-].[Na+].C1(N)C(F)=C(F)C(F)=C(N)C=1F.[ClH:61].Cl>C1COCC1.O>[ClH:40].[ClH:61].[F:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2([CH2:19][CH2:20][CH2:21][N:22]([CH2:24][CH2:25][N:27]3[CH2:28][CH2:29][CH:30]([O:33][C:34]4[CH:35]=[CH:36][C:37]([Cl:40])=[CH:38][CH:39]=4)[CH2:31][CH2:32]3)[CH3:23])[O:15][CH2:16][CH2:17][O:18]2)=[CH:10][CH:9]=1

参加物

8

反応物 5

HCID 14798Sodium HydroxideHCID 71081OxalateHCID 149026Tetrafluoro-m-phenylenediamine dihydrochlorideHCID 202831261-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl}-N-methylaminoacetyl}-4-(4-chlorophenoxy)piperidineHCID 21226445Aluminium lithium hydride

生成物 1

HCID 20283107HCID 20283107、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of 4.68 g of lithium aluminum hydride (61.7 mmol, 50% in oil; washed 3 times with hexane) in 160 ml of THF was added dropwise a solution of 1-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl}-N-methylaminoacetyl}-4-(4-chlorophenoxy)piperidine (liberated from 34.7 g, 0.105 mol, of the oxalate) in 160 ml of dry THF. The mixture was stirred at reflux for 16 hours, allowed to cool to room temperature and subsequently cooled in an ice bath. To the mixture were added slowly, dropwise, 3 ml of water, 3 ml of 15% NaOH and 9 of ml water. The mixture was filtered and the residue washed with THF. Evaporation of the solvent provided an oil. The oil was washed with water, dried over potassium carbonate and the solvent evaporated to provide an oil. The yield of the dihydrochloride was 11.98 g (63%).

後処理

  1. temperatureat reflux for 16 hours
  2. temperaturesubsequently cooled in an ice bath
  3. additionTo the mixture were added slowly
  4. filtrationThe mixture was filtered
  5. washthe residue washed with THF
  6. customEvaporation of the solvent
  7. customprovided an oil
  8. washThe oil was washed with water
  9. dry with materialdried over potassium carbonate
  10. customthe solvent evaporated
  11. customto provide an oil

出典と根拠

ORDレコード
ord-6fa1964ba6764794a09448a348080666
出典データセット
uspto-grants-1985_05
特許番号
US04518713

反応ノート

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