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Trimethylsilylacetylene → HCID 57800198、化合物

HRID 2101866
ノート
印刷プレビュー

反応式

HRID 2101866 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11])=[C:4](I)[C:3]=1[C:16]([F:19])([F:18])[F:17].[Si:20]([C:24]#[CH:25])([CH3:23])([CH3:22])[CH3:21]>[Cu](I)I.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C(N(CC)CC)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11])=[C:4]([C:25]#[C:24][Si:20]([CH3:23])([CH3:22])[CH3:21])[C:3]=1[C:16]([F:19])([F:18])[F:17]
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 2

HCID 66111TrimethylsilylacetyleneHCID 57800179HCID 57800179、化合物

生成物 1

HCID 57800198HCID 57800198、化合物

試薬・触媒・溶媒 3

HCID 83717Copper iodide触媒HCID 178418476HCID 178418476、化合物触媒HCID 8471Triethylamine溶媒

反応条件

温度
50 °C

実験手順

A triethylamine (2.2 mL) solution of N-[4-chloro-2-iodo-3-(trifluoromethyl)phenyl]-2,2-dimethylpropanamide (0.413 g, 1.02 mmol) was treated with TMS acetylene (0.158 mL, 1.12 mmol) followed by copper iodide (0.019 g, 0.102 mmol) and PdCl2(PPh3)2 (0.021 g, 0.031 mmol). The reaction vessel was purged with N2, sealed and heated to 50° C. for 14 h. TLC at this time showed excellent conversion to the desired product. The cooled mixture was filtered through a plug of celite and partitioned between EtOAc (10 mL) and H2O (10 mL). The organic portion was dried (Na2SO4), filtered, and concentrated. Column chromatography (SiO2, EtOAc/hexanes) afforded the title compound as a light brown solid: 1H NMR (CDCl3) δ 8.72 (bs, 1H), 8.64 (d, J=6.0 Hz, 1H), 7.41 (d, J=6.0 Hz, 1H), 1.34 (s, 9H), 0.29 (s, 9H).

後処理

  1. customThe reaction vessel was purged with N2
  2. customsealed
  3. filtrationThe cooled mixture was filtered through a plug of celite
  4. custompartitioned between EtOAc (10 mL) and H2O (10 mL)
  5. dry with materialThe organic portion was dried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-0b93978dcb34454a9b8607bc7b952279
出典データセット
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07572820B2

反応ノート

読み込み中…

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