O-Xylene → HCID 86737387、化合物

HRID 1732726

反応式

HRID 1732726 の反応式
[CH2:1]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:2]([C:12]([O:14][CH2:15][CH3:16])=[O:13])([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:3][CH2:4][CH2:5][CH3:6].[CH2:22]([N:29]1[C:34]([CH3:36])([CH3:35])CC(O)[CH2:31][C:30]1([CH3:39])[CH3:38])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.[C:40]1([CH3:47])[C:41](C)=[CH:42][CH:43]=[CH:44][CH:45]=1.[Li]N>C(O)C>[CH2:22]([N:29]1[C:30]([CH3:38])([CH3:39])[CH2:31][CH:20]([O:19][C:17]([CH2:1][C:2]([C:12]([O:14][CH:15]2[CH2:31][C:30]([CH3:39])([CH3:38])[N:29]([CH2:47][C:40]3[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=3)[C:34]([CH3:36])([CH3:35])[CH2:16]2)=[O:13])([C:7]([O:9][CH:10]2[CH2:39][C:30]([CH3:31])([CH3:38])[N:29]([CH2:22][C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=3)[C:34]([CH3:35])([CH3:36])[CH2:11]2)=[O:8])[CH2:3][CH2:4][CH2:5][CH3:6])=[O:18])[CH2:21][C:34]1([CH3:35])[CH3:36])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

参加物

6

反応物 4

HCID 7237O-XyleneHCID 1036024-Piperidinol, 2,2,6,6-tetramethyl-1-(phenylmethyl)-HCID 122968851,2,2-Hexanetricarboxylic acid, triethyl esterHCID 178506930HCID 178506930、化合物

生成物 1

HCID 86737387HCID 86737387、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

30.2 g (0.1 mol) of triethyl hexane-1,2,2-tricarboxylate, 74.2 g (0.3 mol) of 1-benzyl-2,2,6,6-tetramethyl-4-hydroxypiperidine and 50 ml of xylene are warmed to 130° and mixed with 0.8 g of LiNH2. The ethanol formed is distilled off continuously. The solution is kept at the above temperature for 3 hours, so that it can then be kept at 150° for a further 2 hours. After cooling, the residue is taken up in toluene, a little glacial acetic acid is added to the solution and the latter is washed with H2O. After drying over Na2SO4, the solvent is distilled off in vacuo. Tris-(1-benzyl-2,2,6,6-tetramethyl-4-piperidinyl)hexane-1,2,2-tricarboxylate is obtained as a powdery residue. (Compound No. 1).

後処理

  1. distillationis distilled off continuously
  2. waitcan then be kept at 150° for a further 2 hours
  3. temperatureAfter cooling
  4. additiona little glacial acetic acid is added to the solution
  5. washthe latter is washed with H2O
  6. dry with materialAfter drying over Na2SO4
  7. distillationthe solvent is distilled off in vacuo

出典と根拠

ORDレコード
ord-f49222781930484c9ba96ee7d95aca35
出典データセット
uspto-grants-1980_12
特許番号
US04238613

関連ノート

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