1,2,3,6,-tetrahydro-N-(2-hydroxyethyl)phthalimide → HCID 10896667、化合物

HRID 1422265ノート

反応式

HRID 1422265 の反応式
[OH:1][CH2:2][CH2:3][N:4]1[C:8](=[O:9])[CH:7]2[CH2:10][CH:11]=[CH:12][CH2:13][CH:6]2[C:5]1=[O:14].[C:15]([O:30]CC(C)C)(=O)[CH:16]1[CH2:28][CH:27]=[CH:26][CH2:25][CH:17]1[C:18]([O:20][CH2:21][CH:22](C)C)=[O:19]>[O-]CCCC.[O-]CCCC.[O-]CCCC.[O-]CCCC.[Ti+4].O>[C:18]([O:20][CH2:21][CH2:22][N:4]1[C:5](=[O:14])[CH:6]2[CH2:13][CH:12]=[CH:11][CH2:10][CH:7]2[C:8]1=[O:9])(=[O:19])[CH:17]1[CH2:25][CH:26]=[CH:27][CH2:28][CH:16]1[C:15]([O:1][CH2:2][CH2:3][N:4]1[C:8](=[O:9])[CH:7]2[CH2:10][CH:11]=[CH:12][CH2:13][CH:6]2[C:5]1=[O:14])=[O:30]

参加物

5

反応物 2

HCID 858511,2,3,6,-tetrahydro-N-(2-hydroxyethyl)phthalimideHCID 6432739Diisobutyl 1,2,3,6-tetrahydrophthalate

生成物 1

HCID 10896667HCID 10896667、化合物収率 101%

試薬・触媒・溶媒 2

HCID 21801Titanium tetrabutoxide触媒HCID 962Water溶媒

反応条件

温度
230 °C

実験手順

N-(2-Hydroxyethyl)-1,2,3,6-tetrahydrophthalimide (195.2 g, 1 mol) was dissolved in diisobutyl 1,2,3,6-tetrahydrophthalate (141.2 g, 0.5 mol). The mixture was kept at 150° C. under vacuum to eliminate any traces of water. Titanium tetrabutoxide (1.7 g) was added under atmospheric pressure and the transesterification reaction was carried out distilling off the isobutyl alcohol formed. As the reaction proceeded the temperature was increased stepwise to 230° C. and the pressure was lowered to 20 Torr (26.7 mbar). After ca. 24 h, 265 g of brown crude bis[2-(1,2,3,6-tetrahydrophthalimido)ethyl] 1,2,3,6-tetrahydrophthalate were obtained.

後処理

  1. customwas kept at 150° C. under vacuum
  2. customthe transesterification reaction
  3. distillationwas carried out distilling off the isobutyl alcohol
  4. customformed

出典と根拠

ORDレコード
ord-2ed3f2956efc461882cb3ca99b5c14d4
出典データセット
uspto-grants-2000_06
特許番号
US06080872

反応ノート

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