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Trifluoroacetic acid → N-[2-(Diethylamino)ethyl]-3-[2-(1-naphthyl)ethoxy]-N-(2-oxoethyl)propanamide

HRID 556718
ノート
印刷プレビュー

反応式

HRID 556718 の反応式
[CH2:1]([N:3]([CH2:30][CH3:31])[CH2:4][CH2:5][N:6]([CH2:24][CH:25](OC)[O:26]C)[C:7](=[O:23])[CH2:8][CH2:9][O:10][CH2:11][CH2:12][C:13]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH:16]=[CH:15][CH:14]=1)[CH3:2].FC(F)(F)C(O)=O>C(Cl)Cl>[CH2:30]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][N:6]([CH2:24][CH:25]=[O:26])[C:7](=[O:23])[CH2:8][CH2:9][O:10][CH2:11][CH2:12][C:13]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH:16]=[CH:15][CH:14]=1)[CH3:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 59296255N-[2-(diethylamino)ethyl]-N-(2,2-dimethoxyethyl)-3-[2-(1-naphthyl)ethoxy]propanamide

生成物 1

HCID 59296239N-[2-(Diethylamino)ethyl]-3-[2-(1-naphthyl)ethoxy]-N-(2-oxoethyl)propanamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of N-[2-(diethylamino)ethyl]-N-(2,2-dimethoxyethyl)-3-[2-(1-naphthyl)ethoxy]propanamide (93 g) in DCM (270 mL) was treated dropwise at 0° C. with trifluoroacetic acid (270 mL) over 1.5 hours. After the addition the reaction mixture was allowed to warm to room temperature and stirred for a further 1 hour. The reaction mixture was concentrated and the residue poured into aqueous saturated sodium bicarbonate solution (1800 mL, caution). The aqueous mixture was extracted with DCM (4×400 mL) and the combined extracts were dried over magnesium sulphate and concentrated. The residue was used directly in the following reaction.

後処理

  1. additionAfter the addition the reaction mixture
  2. concentrationThe reaction mixture was concentrated
  3. additionthe residue poured into aqueous saturated sodium bicarbonate solution (1800 mL, caution)
  4. extractionThe aqueous mixture was extracted with DCM (4×400 mL)
  5. dry with materialthe combined extracts were dried over magnesium sulphate
  6. concentrationconcentrated
  7. customThe residue was used directly in the following reaction

出典と根拠

ORDレコード
ord-0f9d3db6d1d04532b23a615b5ec8bd71
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08058294B2

反応ノート

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