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1-Butanol → 4,7-bis(4-isobutoxyphenyl)-2-octyl-2H-benzo[d][1,2,3]triazole

HRID 1050705
ノート
印刷プレビュー

反応式

HRID 1050705 の反応式
Br[C:2]1[C:10]2[C:6](=[N:7][N:8]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[N:9]=2)[C:5](Br)=[CH:4][CH:3]=1.[CH2:20]([O:24][C:25]1[CH:30]=[CH:29][C:28](B(O)O)=[CH:27][CH:26]=1)[CH:21]([CH3:23])[CH3:22].[C:34](=[O:37])([O-])[O-].[Na+].[Na+].[C:40]1(C)[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1.[CH2:47](O)[CH2:48][CH2:49]C>O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:20]([O:24][C:25]1[CH:30]=[CH:29][C:28]([C:2]2[C:10]3[C:6](=[N:7][N:8]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[N:9]=3)[C:5]([C:40]3[CH:41]=[CH:42][C:43]([O:37][CH2:34][CH:48]([CH3:49])[CH3:47])=[CH:44][CH:45]=3)=[CH:4][CH:3]=2)=[CH:27][CH:26]=1)[CH:21]([CH3:23])[CH3:22]
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 5

HCID 2631-ButanolHCID 1140TolueneHCID 10340Sodium CarbonateHCID 162177734-Isobutoxyphenylboronic acidHCID 717214984,7-Dibromo-2-octyl-2H-benzotriazole

生成物 1

HCID 866799224,7-bis(4-isobutoxyphenyl)-2-octyl-2H-benzo[d][1,2,3]triazole

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒
HCID 962Water溶媒2 回

反応条件

温度
105 °C

実験手順

A mixture of Intermediate L (778 mg, 2.0 mmol), 4-isobutoxyphenylboronic acid (970 mg, 5.0 mmol), tetrakis(triphenylphosphine)palladium(0) (500 mg, 0.43 mmol), solution of sodium carbonate (2.12 g, 20 mmol) in water (15 mL), butanol (50 mL), and toluene (30 mL) was vigorously stirred and heated under argon at 105° C. for 16 hours. The reaction mixture was poured into water (200 mL), stirred for 30 minutes and extracted with toluene/ethyl acetate/hexane (2:1:1, 400 mL). The extract was dried over magnesium sulfate, the volatiles were removed under reduced pressure, and the residue was chromatographed (silica gel, hexane/dichloromethane, 1:1). The separated product was crystallized from acetonitrile to give pure 4,7-bis(4-isobutoxyphenyl)-2-octyl-2H-benzo[d][1,2,3]triazole, Compound 45 (1.57 g, 62% yield). 1H NMR (400 MHz, CDCl3): δ 7.99 (d, J=8.8 Hz, 4H, 4-i-BuOC6H4), 7.54 (s, 2H, benzotriazole), 7.04 (d, J=8.8 Hz, 4H, 4-i-BuOC6H4), 4.76 (t, J=7.0 Hz, 2H, octyl), 3.79 (d, J=6.2 Hz, 4H, 4-i-BuOC6H4), 2.13 (m, 4H, octyl), 1.28 (m, 2H, octyl), 1.25 (m, 6H, octyl), 1.04 (d, J=6.6 Hz, 12H, 4-i-BuOC6H4), 0.86 (t, J=6.6 Hz, 3H, octyl). UV-vis spectrum (PVB): λmax=359 nm. Fluorimetry (PVB): λmax=431 nm.

後処理

  1. stirringstirred for 30 minutes
  2. extractionextracted with toluene/ethyl acetate/hexane (2:1:1, 400 mL)
  3. dry with materialThe extract was dried over magnesium sulfate
  4. customthe volatiles were removed under reduced pressure
  5. customthe residue was chromatographed (silica gel, hexane/dichloromethane, 1:1)
  6. customThe separated product was crystallized from acetonitrile

出典と根拠

ORDレコード
ord-617e33f6ca77489eb2e5b45ddd7668c6
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09382424B2

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