O-Xylene → HCID 86737387, 화합물

HRID 1732726

반응식

HRID 1732726 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 86737387HCID 86737387, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-f49222781930484c9ba96ee7d95aca35
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04238613

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