Triethylamine hydrochloride → 5-(4-Chlorobenzyl)-2,2-dimethylcyclopentanone

HRID 1500148노트

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HRID 1500148 반응식
COC([C:5]1([CH2:13][C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)[CH2:9][CH2:8][C:7]([CH3:11])([CH3:10])[C:6]1=[O:12])=O.CN(C)C(=O)C.Cl.C(N(CC)CC)C.O.C(=O)(O)[O-].[Na+]>C1(C)C=CC=CC=1>[Cl:20][C:17]1[CH:16]=[CH:15][C:14]([CH2:13][CH:5]2[C:6](=[O:12])[C:7]([CH3:11])([CH3:10])[CH2:8][CH2:9]2)=[CH:19][CH:18]=1

참가 물질

6

반응물 4

HCID 11130Triethylamine hydrochlorideHCID 31374DimethylacetamideHCID 11449298HCID 11449298, 화합물HCID 86585896Sodium bicarbonate water

생성물 1

HCID 114248965-(4-Chlorobenzyl)-2,2-dimethylcyclopentanone

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
150 °C

실험 절차

In 1-(4-chlorobenzyl)-3,3-dimethyl-2-oxocyclopentane carboxylic acid methyl ester (1.0 g, 0.00339 mol), N,N-dimethylacetamide (1 mL) and triethylamine hydrochloride (0.56 g, 0.00339×1.2 mol) were added and stirred at 150° C. for 2 hours. In the reaction liquid, toluene and saturated sodium bicarbonate water were added, and the mixture was partitioned. After extracting the aqueous layer using toluene, the organic layer was dried using anhydrous sodium sulfate and concentrated. Thereafter, the dried and concentrated product was purified using a silica gel column, and a target product was obtained.

후처리

  1. additionwere added
  2. customthe mixture was partitioned
  3. extractionAfter extracting the aqueous layer
  4. customthe organic layer was dried
  5. concentrationconcentrated
  6. customThereafter, the dried
  7. customconcentrated product was purified
  8. customa target product was obtained

출처 및 근거

ORD 기록
ord-a77e6e71ec454d0ca4206654b4b546b0
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09206106B2

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