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Hydrochloric Acid → HCID 54527635、化合物

HRID 1701105
ノート
印刷プレビュー

反応式

HRID 1701105 の反応式
[CH2:1]([C:3]1([CH3:22])[CH:8]([CH3:9])[CH:7]([NH:10][C:11](=[O:18])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:6][C:5]([CH2:20][CH3:21])([CH3:19])[NH:4]1)[CH3:2].Cl.[CH2:24]1[O:26][CH2:25]1>CO>[OH:26][CH2:25][CH2:24][N:4]1[C:5]([CH2:20][CH3:21])([CH3:19])[CH2:6][CH:7]([NH:10][C:11](=[O:18])[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:8]([CH3:9])[C:3]1([CH2:1][CH3:2])[CH3:22]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 6354Ethylene OxideHCID 22486017N-(2,6-Diethyl-2,3,6-trimethylpiperidin-4-yl)benzamide

生成物 1

HCID 54527635HCID 54527635、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
130 °C

実験手順

30.3 g of 2,6-diethyl-2,3,6-trimethyl-4-benzamidopiperidine (compound no. 9), 200 ml of methanol and 2 ml of concentrated hydrochloric acid are introduced into an autoclave. About 9 g of ethyleneoxide are added, and the contents of the autoclave are heated to 130° C. for 30 hours. After cooling, the contents of the autoclave are purified by filtration, and the methanol is evaporated. Crystallization of the residue from toluene yields 1-β-hydroxyethyl-2,6-diethyl-2,3,6-trimethyl-4-benzamidopiperidine (compound no. 27); m.p. 212°-214° C. If, instead of 30.3 g of 2,6-diethyl-2,3,6-trimethyl-4-benzamidopiperidine an equimolar amount of N,N'-diacetyl-N,N'-bis-(2,6-diethyl-2,3,6-trimethyl-4-piperidyl)-hexamethylene-1,6-diamine (compound no. 22), 12 g instead of 9 g of ethyleneoxide are used and otherwise the procedure described above is followed, N,N'-diacetyl-N,N'-bis-(1-β-hydroxyethyl-2,6-diethyl-2,3,6-trimethyl-4-piperidyl)-hexamethylene-1,6-diamine (compound no. 28) is obtained as a yellowish viscous resin.

後処理

  1. temperatureAfter cooling
  2. filtrationthe contents of the autoclave are purified by filtration
  3. customthe methanol is evaporated
  4. customCrystallization of the residue from toluene

出典と根拠

ORDレコード
ord-616ba2544c5b4ec98879ce4fb1f4a6ec
出典データセット
uspto-grants-1980_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04191683

反応ノート

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