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2-Dimethylaminopyridine → (Trimethylsilyl)ethyl 4-[(5,6,7,8-tetrahydro-8,8-dimethyl-5-oxonaphth-2-yl)ethynyl]benzoate

HRID 1238
ノート
印刷プレビュー

反応式

HRID 1238 の反応式
[CH3:1][C:2]1([CH3:24])[C:11]2[CH:10]=[C:9]([C:12]#[C:13][C:14]3[CH:22]=[CH:21][C:17]([C:18]([OH:20])=[O:19])=[CH:16][CH:15]=3)[CH:8]=[CH:7][C:6]=2[C:5](=[O:23])[CH2:4][CH2:3]1.CN(C1C=CC=CN=1)C.[CH3:34][Si:35]([CH:38](O)[CH3:39])([CH3:37])[CH3:36].Cl.CN(C)CCCN=C=NCC>C(Cl)Cl>[CH3:1][C:2]1([CH3:24])[C:11]2[CH:10]=[C:9]([C:12]#[C:13][C:14]3[CH:15]=[CH:16][C:17]([C:18]([O:20][CH2:39][CH2:38][Si:35]([CH3:37])([CH3:36])[CH3:34])=[O:19])=[CH:21][CH:22]=3)[CH:8]=[CH:7][C:6]=2[C:5](=[O:23])[CH2:4][CH2:3]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 218852-DimethylaminopyridineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 124478981-(Trimethylsilyl)ethanolHCID 153455474-((5,6,7,8-Tetrahydro-8,8-dimethyl-5-oxonaphth-2-yl)ethynyl]benzoic acid2 回

生成物 1

HCID 54412444(Trimethylsilyl)ethyl 4-[(5,6,7,8-tetrahydro-8,8-dimethyl-5-oxonaphth-2-yl)ethynyl]benzoate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

To a solution of 0.24 g (0.73 mmol) of 4-[(5,6,7,8-tetrahydro-8,8-dimethyl-5-oxonaphth-2-yl)ethynyl]benzoic acid (Compound 7) in 10 ml of dry CH2Cl2 was added 0.09 g (0.74 mmol) of dimethylaminopyridine, 0.115 ml (0.80 mmol) of trimethylsilylethanol and 0.17 g (0.88 mmol) of 1-(3-dimethylaminopropyl)-3-ethyl carbodiimide hydrochloride. The reaction mixture was stirred at 25° C. for 5 hours, washed with sat. aqueous NaHCO3 and brine, dried over Na2SO4 and concentrated in vacuo to an oil. Purification by flash chromatography (silica, 10% EtOAc-hexane) yielded the title compound as a white solid.

後処理

  1. washwashed with sat. aqueous NaHCO3 and brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated in vacuo to an oil
  4. customPurification by flash chromatography (silica, 10% EtOAc-hexane)

出典と根拠

ORDレコード
ord-558960f60108438697a2928369019551
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05723620

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート