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Sodium Carbonate → HCID 18982655、化合物

HRID 1707208
ノート
印刷プレビュー

反応式

HRID 1707208 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6](B(O)O)=[CH:5][CH:4]=1)#[N:2].[CH2:12]([S:19][C:20]1[CH:25]=[CH:24][C:23](Br)=[CH:22][CH:21]=1)[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:23]2[CH:24]=[CH:25][C:20]([S:19][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[CH:21][CH:22]=2)=[CH:5][CH:4]=1)#[N:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 27343264-Cyanophenylboronic acidHCID 12521245Benzene, 1-bromo-4-(heptylthio)-

生成物 1

HCID 18982655HCID 18982655、化合物収率 30%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

4-Cyanophenylboronic acid (7 g, 0.0476 m) was stirred and refluxed for 60 hours under nitrogen with 4-n-heptylthiobromobenzene (12.4 g, 0.0433 m), TTPP (0.9 g, 0.000783 m), 2 molar aqueous sodium carbonate (41 mls), toluene (86 mls) and industrial methylated spirit (20.5 mls). The mixture was then separated end extincted with toluene (2×10 mls) washed with water (100 mls) and dried over magnesium sulphate. The solvents were then evaporated off to give a brown solid products which was purified by column chromatography and recrystallisation from industrial methylated spirit. 4-Cyano-4'-heptylthiobiphenyl was produced (4.1 g, 100% HPCL, 30% yield melting point 64.4° C.).

後処理

  1. customThe mixture was then separated end
  2. washwashed with water (100 mls)
  3. dry with materialdried over magnesium sulphate
  4. customThe solvents were then evaporated off
  5. customto give a brown solid products which
  6. customwas purified by column chromatography and recrystallisation from industrial methylated spirit

出典と根拠

ORDレコード
ord-fbf2878a83214f49ba4bde529b07025e
出典データセット
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05352381

反応ノート

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