ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Triethylamine → (4-Acetoxy-6-fluoro-3-trimethylsilanylethynyl-naphthalen-2-yl)-acetic acid methyl ester

HRID 238641
ノート
印刷プレビュー

反応式

HRID 238641 の反応式
[CH3:1][O:2][C:3](=[O:21])[CH2:4][C:5]1[C:14](I)=[C:13]([O:16][C:17](=[O:19])[CH3:18])[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([F:20])[CH:11]=2)[CH:6]=1.C(N(CC)CC)C.[CH3:29][Si:30]([C:33]#[CH:34])([CH3:32])[CH3:31]>CN(C)C=O.C(OCC)(=O)C.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.[Cu](I)I>[CH3:1][O:2][C:3](=[O:21])[CH2:4][C:5]1[C:14]([C:34]#[C:33][Si:30]([CH3:32])([CH3:31])[CH3:29])=[C:13]([O:16][C:17](=[O:19])[CH3:18])[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([F:20])[CH:11]=2)[CH:6]=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

8

反応物 3

HCID 8471TriethylamineHCID 66111TrimethylsilylacetyleneHCID 59326600(4-Acetoxy-6-fluoro-3-iodo-naphthalen-2-yl)acetic acid methyl ester

生成物 1

HCID 59326569(4-Acetoxy-6-fluoro-3-trimethylsilanylethynyl-naphthalen-2-yl)-acetic acid methyl ester収率 75%

試薬・触媒・溶媒 4

HCID 83717Copper iodide触媒
HCID 178418476
HCID 178418476、化合物
触媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
150 °C

実験手順

To a solution of (4-acetoxy-6-fluoro-3-iodo-naphthalen-2-yl)acetic acid methyl ester (300 mg, 0.75 mmol) and triethylamine (3 mL) in N,N-dimethylformamide (3 mL), was added bis(triphenylphosphine)dichloropalladium(II) (53 mg, 0.075 mmol), copper iodide (42 mg, 0.229 mmol) and trimethylsilanylacetylene (108 mg, 1.12 mmol) under an argon atmosphere. After being heated at 150° C. for 6 minutes with microwave irradiation, the resulting mixture was cooled, diluted with ethyl acetate (20 mL), and washed with brine (15 mL×2). The organic layer was dried over sodium sulfate and concentrated in vacuo. The residue was purified by flash column (elution with 10% ethyl acetate in petroleum ether) to afford (4-acetoxy-6-fluoro-3-trimethylsilanylethynyl-naphthalen-2-yl)-acetic acid methyl ester (208 mg, 75%) as a light yellow solid.

後処理

  1. temperaturethe resulting mixture was cooled
  2. washwashed with brine (15 mL×2)
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash column (elution with 10% ethyl acetate in petroleum ether)

出典と根拠

ORDレコード
ord-02522059d1f24a22adafe5a74d46d339
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08642629B2

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