Dibutyltin oxide → HCID 178418280、化合物

HRID 1625

反応式

HRID 1625 の反応式
[O:1]([C:8]1[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([Sn](=O)CCCC)CCC.C[Si]([N:30]=[N+:31]=[N-:32])(C)C>C1(C)C=CC=CC=1>[O:1]([C:8]1[CH:9]=[CH:10][C:11]([C:12]2[NH:32][N:31]=[N:30][N:13]=2)=[CH:14][CH:15]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 61221Dibutyltin oxideHCID 78378AzidotrimethylsilaneHCID 1378214-Phenoxybenzonitrile

生成物 1

HCID 178418280HCID 178418280、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 4-phenoxybenzonitrile (9.87 g), dibutyltin oxide (3.88 g), and trimethylsilyl azide (33.5 ml) in anhydrous toluene (200 ml) was heated to reflux for 6 hours. The reaction mixture was washed with 1.6M sodium hydroxide (2×250 ml). The combined aqueous layer was washed with diethyl ether (4×120 ml) then acidified to pH 6 with concentrated hydrochloric acid. The acidic solution was washed with ethyl acetate (3×200 ml) and the combined organic layer was dried over anhydrous sodium sulfate, filtered and evaporated to dryness to give 5-(4-phenoxyphenyl)-1H-tetrazole as a white powder.

後処理

  1. temperatureto reflux for 6 hours
  2. washThe reaction mixture was washed with 1.6M sodium hydroxide (2×250 ml)
  3. washThe combined aqueous layer was washed with diethyl ether (4×120 ml)
  4. washThe acidic solution was washed with ethyl acetate (3×200 ml)
  5. dry with materialthe combined organic layer was dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-ffa107eae87c458391df6e58d5d78f6e
出典データセット
uspto-grants-1998_03
特許番号
US05726195

関連ノート

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