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4-trimethylsilylaniline → 12,12-Difluorododec-11-enoic acid N-(4-trimethylsilylphenyl)amide

HRID 1077706
ノート
印刷プレビュー

反応式

HRID 1077706 の反応式
CO[C:3](=[O:17])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH:13]=[C:14]([F:16])[F:15].[CH3:18][Si:19]([CH3:28])([CH3:27])[C:20]1[CH:26]=[CH:25][C:23]([NH2:24])=[CH:22][CH:21]=1>C1(C)C=CC=CC=1>[CH3:18][Si:19]([CH3:28])([CH3:27])[C:20]1[CH:26]=[CH:25][C:23]([NH:24][C:3](=[O:17])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH:13]=[C:14]([F:15])[F:16])=[CH:22][CH:21]=1
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 100349574-trimethylsilylanilineHCID 11149322Methyl 12,12-difluoro-11-dodecenoate

生成物 1

HCID 1791256312,12-Difluorododec-11-enoic acid N-(4-trimethylsilylphenyl)amide

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

2.5 g of 12,12-difluorododec-11-enoic acid methyl ester are added at room temperature to 1.53 g of 4-trimethylsilylaniline in 25 ml of toluene. The mixture is stirred for 2 hours at 80° and then concentrated by evaporation in vacuo. The residue is taken up in toluene, the toluene phase is washed with water, dried over sodium sulfate and concentrated to dryness by evaporation. The residue is taken up in hexane:ethyl acetate (9:1) and filtered over silica gel. Evaporation of the filtrate yields the title compound (nD24 =1.5038; compound no. 1-2).

後処理

  1. concentrationconcentrated by evaporation in vacuo
  2. washthe toluene phase is washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated to dryness by evaporation
  5. filtrationfiltered over silica gel
  6. customEvaporation of the filtrate

出典と根拠

ORDレコード
ord-4aae1c82fbe04728bea68575e8343b34
出典データセット
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05545630

反応ノート

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