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Triethylamine → 5-fluoro-1-methyl-3-(tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-indole

HRID 2362706
ノート
印刷プレビュー

反応式

HRID 2362706 の反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH3:11])[CH:6]=[C:5]2I.C(N(CC)CC)C.[CH3:20][C:21]1([CH3:28])[C:25]([CH3:27])([CH3:26])[O:24][BH:23][O:22]1>O1CCOCC1.C(OCC)(=O)C.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].ClCCl>[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH3:11])[CH:6]=[C:5]2[B:23]1[O:24][C:25]([CH3:27])([CH3:26])[C:21]([CH3:28])([CH3:20])[O:22]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

7

反応物 3

HCID 8471TriethylamineHCID 27347684,4,5,5-Tetramethyl[1,3,2]dioxaborolaneHCID 670034715-fluoro-3-iodo-1-methyl-1H-indole

生成物 1

HCID 670035225-fluoro-1-methyl-3-(tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-indole

試薬・触媒・溶媒 3

HCID 178418807HCID 178418807、化合物触媒
HCID 8857
Ethyl Acetate
溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

A solution of 5-fluoro-3-iodo-1-methyl-1H-indole (11.5 g, 41.8 mmol) in dioxane (200 mL) was treated with triethyl amine (27 mL, 194 mmol) and [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) dichloromethane (1.707 g, 2.090 mmol). 4,4,5,5-Tetramethyl-1,3,2-dioxaborolane (39.4 mL, 272 mmol) was added carefully to the reaction (gas evolution was observed). The mixture was heated to 100° C. for 30 minutes, cooled, and diluted with about 250 mL ethyl acetate. The precipitate was filtered and washed with ethyl acetate (100 mL). The filtrate was concentrated under reduced pressure. The residue was purifed on silica gel, eluting with 8:2 heptane:ethyl acetate, to give the title compound. MS ESI(+) m/z 276.0 (M+H)+.

後処理

  1. temperaturecooled
  2. filtrationThe precipitate was filtered
  3. washwashed with ethyl acetate (100 mL)
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. washeluting with 8:2 heptane

出典と根拠

ORDレコード
ord-b21849c451914a7aac59fac3bad305a2
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08691810B2

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