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4,4,5,5-Tetramethyl[1,3,2]dioxaborolane → 5-methoxy-1-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-indole

HRID 1628016
ノート
印刷プレビュー

反応式

HRID 1628016 の反応式
I[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([O:11][CH3:12])[CH:9]=2)[N:4]([CH3:13])[CH:3]=1.[CH3:14][C:15]1([CH3:22])[C:19]([CH3:21])([CH3:20])[O:18][BH:17][O:16]1>O1CCOCC1.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].C(Cl)Cl>[CH3:12][O:11][C:8]1[CH:9]=[C:10]2[C:5](=[CH:6][CH:7]=1)[N:4]([CH3:13])[CH:3]=[C:2]2[B:17]1[O:18][C:19]([CH3:21])([CH3:20])[C:15]([CH3:22])([CH3:14])[O:16]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

5

反応物 2

HCID 27347684,4,5,5-Tetramethyl[1,3,2]dioxaborolaneHCID 534021023-Iodo-5-methoxy-1-methyl-1H-indole

生成物 1

HCID 580098415-methoxy-1-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-indole収率 37.3%

試薬・触媒・溶媒 2

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

反応条件

温度
100 °C

実験手順

The 3-iodo-5-methoxy-1-methyl-1H-indole (9.90 g, 34.5 mmol) in 1,4-dioxane (200 mL) was treated with PdCl2(dppf)-CH2Cl2 (1.41 g, 1.72 mmol), TEA (33.6 mL, 241 mmol) and 4,4,5,5-tetramethyl-1,3,2-dioxaborolane (28.7 g, 224 mmol). The mixture was heated to about 100° C. for about 40 min. The mixture was cooled to rt and concentrated under reduced pressure. The material was stirred with EtOAc (300 mL) at rt for about 30 min and then filtered. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel chromatography eluting with 100% DCM to give 5-methoxy-1-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-indole (3.7 g, 37%): LC/MS (Table 2, Method a) Rt=2.68 min; MS m/z 288 (M+H)+.

後処理

  1. temperatureThe mixture was cooled to rt
  2. concentrationconcentrated under reduced pressure
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customthe residue was purified by silica gel chromatography
  6. washeluting with 100% DCM

出典と根拠

ORDレコード
ord-94d65d28218b4939b3c2a52395f322dd
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08785639B2

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