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Dicyclohexylcarbodiimide → HCID 19857803、化合物

HRID 1902220
ノート
印刷プレビュー

反応式

HRID 1902220 の反応式
C1(N=C=NC2CCCCC2)CCCCC1.[CH2:16]([CH:21]([CH:25]([OH:32])[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])[C:22]([OH:24])=[O:23])[CH2:17][CH2:18][CH2:19][CH3:20].O[N:34]1[C:38](=[O:39])[CH2:37][CH2:36][C:35]1=[O:40]>COCCOC>[CH2:16]([CH:21]([CH:25]([OH:32])[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])[C:22]([OH:24])=[O:23])[CH2:17][CH2:18][CH2:19][CH3:20].[C:35]1(=[O:40])[NH:34][C:38](=[O:39])[CH2:37][CH2:36]1
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 10868DicyclohexylcarbodiimideHCID 80170N-HydroxysuccinimideHCID 19857780HCID 19857780、化合物

生成物 1

HCID 19857803HCID 19857803、化合物収率 104.2%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒2 回

反応条件

温度
0 °C

実験手順

Dicyclohexylcarbodiimide (27 g) dissolved in 1,2-dimethoxyethane (300 cc) is added, in the course of 40 minutes, to a solution, kept at 0° C., of 2-n-pentyl-3-hydroxynonanoic acid (29.1 g) and N-hydroxysuccinimide (14.1 g) in 1,2-dimethoxyethane (300 cc). The reaction mixture is stirred at 0° C. for 3 hours and then kept at 4° C. for 21 hours. The precipitate formed is filtered off and washed twice with 1,2-dimethoxyethane (100 cc in total). The filtrate is concentrated to dryness under reduced pressure (20 mm Hg) at 50° C. The concentrate is taken up in a mixture of diisopropyl ether (300 cc) and acetic acid (3 cc). After standing for 2 hours at 20° C., the precipitate formed is filtered off and washed twice with diisopropyl ether (40 cc in total). The filtrate is concentrated to dryness under reduced pressure (20 mm Hg) at 50° C. Succinimide 2-n-pentyl-3-hydroxynonanoate (42.6 g) is thus obtained in the form of a yellow oil.

後処理

  1. additionis added, in the course of 40 minutes, to a solution
  2. waitkept at 4° C. for 21 hours
  3. customThe precipitate formed
  4. filtrationis filtered off
  5. washwashed twice with 1,2-dimethoxyethane (100 cc in total)
  6. concentrationThe filtrate is concentrated to dryness under reduced pressure (20 mm Hg) at 50° C
  7. additionThe concentrate is taken up in a mixture of diisopropyl ether (300 cc) and acetic acid (3 cc)
  8. waitAfter standing for 2 hours at 20° C.
  9. customthe precipitate formed
  10. filtrationis filtered off
  11. washwashed twice with diisopropyl ether (40 cc in total)
  12. concentrationThe filtrate is concentrated to dryness under reduced pressure (20 mm Hg) at 50° C

出典と根拠

ORDレコード
ord-6cae515619a748c8921fbbabb2e435bf
出典データセット
uspto-grants-1982_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04362716

反応ノート

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