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Triethylamine → [6-[[(2-Piperidinoethyl)amino]carbonyl]-3-cyclohexenyl]methyl N-octadecylcarbamate

HRID 566427
ノート
印刷プレビュー

反応式

HRID 566427 の反応式
C(N(CC)CC)C.[CH2:8]([N:26]=[C:27]=[O:28])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25].[OH:29][CH2:30][CH:31]1[CH:36]([C:37]([NH:39][CH2:40][CH2:41][N:42]2[CH2:47][CH2:46][CH2:45][CH2:44][CH2:43]2)=[O:38])[CH2:35][CH:34]=[CH:33][CH2:32]1>C(Cl)Cl>[CH2:8]([NH:26][C:27](=[O:28])[O:29][CH2:30][CH:31]1[CH:36]([C:37]([NH:39][CH2:40][CH2:41][N:42]2[CH2:47][CH2:46][CH2:45][CH2:44][CH2:43]2)=[O:38])[CH2:35][CH:34]=[CH:33][CH2:32]1)[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]
参加物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 8471Triethylamine2 回HCID 66988Octadecyl isocyanate2 回HCID 212661176-(Hydroxymethyl)-N-(2-piperidinoethyl)-3-cyclohexene-1-carboxamide

生成物 1

HCID 21266136[6-[[(2-Piperidinoethyl)amino]carbonyl]-3-cyclohexenyl]methyl N-octadecylcarbamate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Triethylamine (0.96 ml) and octadecyl isocyanate (2.2 ml) were added to a solution of 6-(hydroxymethyl)-N-(2-piperidinoethyl)-3-cyclohexene-1-carboxamide (1.65 g) in methylene chloride (22 ml). After being stirred for 15 hours at room temperature, triethylamine (0.96 ml) and octadecyl isocyanate (2.2 ml) were further added to the reaction mixture and stirred for 5 hours at room temperature. The insoluble matters were filtrated out under a vacuum and washed with chloroform. The filtrate and washings were combined together and the mixture was washed with saturated sodium hydrogencarbonate aqueous solution and saturated brine successively, dried over sodium sulfate anhydride, and concentrated. The residue was purified by silica gel column chromatography (silica gel 100 g, chloroform:methanol=30:1-10:1), thereby yielding the entitled compound (2.59 g) as white solid.

後処理

  1. stirringstirred for 5 hours at room temperature
  2. filtrationThe insoluble matters were filtrated out under a vacuum
  3. washwashed with chloroform
  4. washthe mixture was washed with saturated sodium hydrogencarbonate aqueous solution and saturated brine successively
  5. dry with materialdried over sodium sulfate anhydride
  6. concentrationconcentrated
  7. customThe residue was purified by silica gel column chromatography (silica gel 100 g, chloroform:methanol=30:1-10:1)

出典と根拠

ORDレコード
ord-2b59af2224d042a985fb4e7254dfe2ea
出典データセット
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06174885B1

反応ノート

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