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Triethylamine → HCID 15887790、化合物

HRID 381486
ノート
印刷プレビュー

反応式

HRID 381486 の反応式
CCN=[C:4]=[N:5][CH2:6][CH2:7][CH2:8]N(C)C.Cl.CCN(CC)CC.C1CCC(N=[C:27]=[N:28][CH:29]2[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]2)CC1.[CH:35]1[CH:36]=[CH:37][C:38]2N(O)N=N[C:39]=2[CH:40]=1.[C:45]([NH:48][C:49]1[CH:54]=[CH:53][C:52](/[CH:55]=[CH:56]/[C:57]([OH:59])=O)=[CH:51][CH:50]=1)(=[O:47])[CH3:46]>C(Cl)Cl.C(Cl)Cl.CO>[O:59]=[C:57]([N:5]1[CH2:6][CH2:7][C:8]2[C:30]3[C:29](=[CH:34][CH:33]=[CH:32][CH:31]=3)[NH:28][C:27]=2[CH:4]1[C:39]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:40]=1)/[CH:56]=[CH:55]/[C:52]1[CH:51]=[CH:50][C:49]([NH:48][C:45](=[O:47])[CH3:46])=[CH:54][CH:53]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 8471TriethylamineHCID 10868DicyclohexylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 53571554-Acetamidocinnamic acid

生成物 1

HCID 15887790HCID 15887790、化合物収率 51%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 21226129Dichloromethane methanol溶媒

実験手順

To a solution of Intermediate 1 (0.2 g, 0.81 mmol) in 40 mL of DCM were added Et3N (0.13 mL, 1.1 equiv.), DCC (0.18 g, 1.1 equiv.), HOBT (0.12 g , 1.1 equiv.) and (E)-3-(4-acetylaminophenyl)acrylic acid (0.18 g , 1.1 equiv.). After 24 hours of stirring at rt the reaction was judged to be completed by tlc monitoring (SiO2, DCM:MeOH 95:5) and was quenched with 150 mL of water. A white solid precipitated out and was filtered off. The filtrate was extracted with DCM, washed with brine (5 mL), dried over MgSO4 and concentrated in vacuo. Flash chromatography on a 2.5×25 cm2 column of silica gel using DCM:MeOH (98:2) as eluting solvent and removal of the solvent in vacuo gave the title compound (0.18 g, 51%) as yellow crystals after recrystallization from 2-propanol:pentane.

後処理

  1. customwas quenched with 150 mL of water
  2. customA white solid precipitated out and
  3. filtrationwas filtered off
  4. extractionThe filtrate was extracted with DCM
  5. washwashed with brine (5 mL)
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo
  8. washas eluting
  9. customsolvent and removal of the solvent in vacuo

出典と根拠

ORDレコード
ord-9ba7b5f799864c85942d49708ab47911
出典データセット
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06306870B1

反応ノート

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