4-Piperidinol, 1,2,2,6,6-pentamethyl- → 1,2,2,6,6-Pentamethylpiperidin-4-yl 3-(5-Phenylsulfonylbenzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydrocinnamate

HRID 28328

반응식

HRID 28328 반응식
[C:1]1([S:7]([C:10]2[CH:35]=[CH:34][C:13]3=[N:14][N:15]([C:17]4[CH:18]=[C:19]([CH:26]=[C:27]([C:30]([CH3:33])([CH3:32])[CH3:31])[C:28]=4[OH:29])[CH2:20][CH2:21][C:22]([O:24][CH3:25])=[O:23])[N:16]=[C:12]3[CH:11]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:36][N:37]1[C:42]([CH3:44])([CH3:43])[CH2:41]C(O)[CH2:39][C:38]1([CH3:47])[CH3:46].C([Sn](=O)CCCCCCCC)CCCCCCC>>[C:1]1([S:7]([C:10]2[CH:35]=[CH:34][C:13]3=[N:14][N:15]([C:17]4[CH:18]=[C:19]([CH:26]=[C:27]([C:30]([CH3:32])([CH3:31])[CH3:33])[C:28]=4[OH:29])[CH2:20][CH2:21][C:22]([O:24][CH:25]4[CH2:41][C:42]([CH3:44])([CH3:43])[N:37]([CH3:36])[C:38]([CH3:47])([CH3:46])[CH2:39]4)=[O:23])[N:16]=[C:12]3[CH:11]=2)(=[O:9])=[O:8])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 3

HCID 754724-Piperidinol, 1,2,2,6,6-pentamethyl-HCID 93563Dioctyltin oxideHCID 22595036Methyl 3-(5-phenylsulfonylbenzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydrocinnamate

생성물 1

HCID 101459721,2,2,6,6-Pentamethylpiperidin-4-yl 3-(5-Phenylsulfonylbenzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydrocinnamate수율 70%

반응 조건

온도
160 °C

실험 절차

Methyl 3-(5-phenylsulfonylbenzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydro-cinnamate (5 g, 0.01 mol), xylenes (18 g, 0.17 mol), 1,2,2,6,6-pentamethyl-4-hydroxy-piperidine (2.1 g, 0.012 mol) and dioctyltin oxide (0.5 g, 0.0014 mol) are charged to a reactor and heated to 160° C. while being vigorously stirred. At the end of six hours, any remaining xylene is removed by distillation under vacuum. The crude yellow oil obtained is chromatographed through a pad of silica gel using ethyl aetate as the eluent. The title compound is obtained in a 70% yield as a low melting yellow solid, melting at 45-52° C., whose structure is consistent with 1Hnmr and mass spectrometry.

후처리

  1. customAt the end of six hours, any remaining xylene is removed by distillation under vacuum
  2. customThe crude yellow oil obtained
  3. customis chromatographed through a pad of silica gel

출처 및 근거

ORD 기록
ord-f22f27baf214491bb600c143b331795b
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07419513B2

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