Propylamine → HCID 16736832, 화합물

HRID 1170456노트

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HRID 1170456 반응식
[Cl:1][C:2]1[CH:19]=[CH:18][CH:17]=[CH:16][C:3]=1[C:4]([CH:6]1[C:11](=[O:12])OC(C)(C)OC1=O)=[O:5].[CH2:20]([NH2:23])[CH2:21][CH3:22]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:19]=[CH:18][CH:17]=[CH:16][C:3]=1[C:4](=[O:5])[CH2:6][C:11]([NH:23][CH2:20][CH2:21][CH3:22])=[O:12]

참가 물질

4

반응물 2

HCID 7852PropylamineHCID 167368235-(2-Chlorobenzoyl)-2,2-dimethyl-1,3-dioxane-4,6-dione

생성물 1

HCID 16736832HCID 16736832, 화합물수율 53%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
85 °C

실험 절차

A suspension of 5-(2-chlorobenzoyl)-2,2-dimethyl-1,3-dioxane-4,6-dione (2.06 g, 7.30 mmol) in 100 mL of toluene was treated with neat propylamine (550 μL, 395 mg, 6.70 mmol) added dropwise via syringe. The reaction was then heated at 80-90° C. for 4 h. Once at rt, the reaction was concentrated to dryness. The residue was adsorbed onto flash silica gel and added to 19 cm of flash silica gel in a 5 cm dia. column. Elution with 4:1 hexanes/EtOAc afforded 851 mg (53%) of the title compound as a yellow oil.

후처리

  1. additionadded dropwise via syringe
  2. concentrationOnce at rt, the reaction was concentrated to dryness
  3. additionadded to 19 cm of flash silica gel in a 5 cm dia
  4. washElution with 4:1 hexanes/EtOAc

출처 및 근거

ORD 기록
ord-b2cb57c9322748b48feb004e725fc5fc
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07825278B2

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