1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 66637839、化合物

HRID 1094285ノート

反応式

HRID 1094285 の反応式
[C:1]([O:12][CH3:13])(=[O:11])[C:2]1[CH:10]=[CH:9][CH:8]=[C:4]([C:5]([O-:7])=O)[CH:3]=1.[CH3:14][O:15][CH:16]([O:19][CH3:20])[CH2:17][NH2:18].CCN=C=NCCCN(C)C.CCN(C(C)C)C(C)C>C(Cl)Cl>[CH3:13][O:12][C:1](=[O:11])[C:2]1[CH:10]=[CH:9][CH:8]=[C:4]([C:5]([NH:18][CH2:17][CH:16]([O:19][CH3:20])[O:15][CH3:14])=[O:7])[CH:3]=1

参加物

6

反応物 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 81531DiisopropylethylamineHCID 89728Aminoacetaldehyde dimethyl acetalHCID 69512791,3-Benzenedicarboxylic acid, monomethyl ester

生成物 1

HCID 66637839HCID 66637839、化合物収率 104.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Mono-methyl isophthalate (1 g, 5.55 mmol), amino acetaldehyde dimethyl acetal (569 μL, 5.28 mmol) and EDCI (1.52 g, 7.92 mmol) were dissolved in 55 mL DCM, followed by the addition of DIPEA (1.84 mL, 10.56 mmol). The reaction was allowed to stir at room temperature for 2 hours. It was then taken up in 50 mL of DCM, washed with saturated NaHCO3 solution (100 mL), and brine (100 mL). The organic layer was dried over MgSO4, filtered and concentrated to afford the crude product (1.48 g) as a clear oil which was used in the next step without further purification.

後処理

  1. washwashed with saturated NaHCO3 solution (100 mL), and brine (100 mL)
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-4ee8794b548a4469acabc68fe326b9e0
出典データセット
uspto-grants-2012_03
特許番号
US08133905B2

反応ノート

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