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1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → isopropyl 2-(3-(6-Hexyl-1-naphthamido)phenoxy)acetate

HRID 472783
ノート
印刷プレビュー

反応式

HRID 472783 の反応式
Cl.C(N=C=NCCCN(C)C)C.[CH2:13]([C:19]1[CH:20]=[C:21]2[C:26](=[CH:27][CH:28]=1)[C:25]([C:29]([OH:31])=O)=[CH:24][CH:23]=[CH:22]2)[CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].[NH2:32][C:33]1[CH:34]=[C:35]([CH:44]=[CH:45][CH:46]=1)[O:36][CH2:37][C:38]([O:40][CH:41]([CH3:43])[CH3:42])=[O:39]>C(Cl)Cl>[CH2:13]([C:19]1[CH:20]=[C:21]2[C:26](=[CH:27][CH:28]=1)[C:25]([C:29]([NH:32][C:33]1[CH:34]=[C:35]([CH:44]=[CH:45][CH:46]=1)[O:36][CH2:37][C:38]([O:40][CH:41]([CH3:42])[CH3:43])=[O:39])=[O:31])=[CH:24][CH:23]=[CH:22]2)[CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]
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 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 10608474Isopropyl 2-(3-aminophenoxy)acetateHCID 543973816-Hexyl-1-naphthoic acid

生成物 1

HCID 66660445isopropyl 2-(3-(6-Hexyl-1-naphthamido)phenoxy)acetate収率 23.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1-Ethyl-3-(3′-dimethylaminopropyl)-carbodiimide hydrochloride (EDCI, 157 mg) was added to a solution of 6-hexyl-1-naphthoic acid (161 mg, 0.63 mmol) and isopropyl 2-(3-aminophenoxy)acetate (131 mg, 0.63 mmol) in CH2Cl2 (6.3 mL) and the solution was stirred at room temperature overnight. The reaction was concentrated in vacuo, diluted with water (25 mL) and extracted with EtOAc (2×25 mL). The combined organic phase was washed with 1 N aqueous HCl (20 mL), saturated aqueous NaHCO3 (20 mL) and brine (20 mL), then dried (Na2SO4), filtered and concentrated in vacuo. The crude residue was purified on 40 g silica (100% hexanes→100% EtOAc, gradient) to afford 65 mg (23%) of isopropyl 2-(3-(6-Hexyl-1-naphthamido)phenoxy)acetate.

後処理

  1. concentrationThe reaction was concentrated in vacuo
  2. additiondiluted with water (25 mL)
  3. extractionextracted with EtOAc (2×25 mL)
  4. washThe combined organic phase was washed with 1 N aqueous HCl (20 mL), saturated aqueous NaHCO3 (20 mL) and brine (20 mL)
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe crude residue was purified on 40 g silica (100% hexanes→100% EtOAc, gradient)

出典と根拠

ORDレコード
ord-04577eb0cbab4094956826a2102e533e
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08633220B2

反応ノート

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