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

反応式

HRID 28328 の反応式
[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

参加物

4

反応物 3

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

生成物 1

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

反応条件

温度
160 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f22f27baf214491bb600c143b331795b
出典データセット
uspto-grants-2008_09
特許番号
US07419513B2

関連ノート

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