Sodium Hydroxide → HCID 178418490、化合物

HRID 1629

反応式

HRID 1629 の反応式
[O:1]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][C:15]#[N:16])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C[Si]([N:21]=[N+:22]=[N-:23])(C)C.C([Sn](=O)CCCC)CCC.[OH-].[Na+]>C1(C)C=CC=CC=1>[O:1]([C:8]1[CH:9]=[CH:10][C:11]([CH2:14][C:15]2[NH:23][N:22]=[N:21][N:16]=2)=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 61221Dibutyltin oxideHCID 78378AzidotrimethylsilaneHCID 27779534-Phenoxyphenylacetonitrile

生成物 1

HCID 178418490HCID 178418490、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a solution of 4-phenoxyphenylacetonitrile (1.16 g) in anhydrous toluene (30 ml) was added trimethylsilylazide (1.1 ml) and dibutyltin oxide (0.19 g). The mixture was heated to reflux for 19 hours then allowed to cool to room temperature. The reaction mixture was then added to 1M sodium hydroxide (100 ml) and washed with diethyl ether (3×50 ml). The aqueous layer was acidified with concentrated hydrochloric acid (30 ml) then washed with 5:1 ethyl acetate/tetrahydrofuran (60 ml) and ethyl acetate (2×50 ml). The combined organic layer was dried over anhydrous sodium sulfate, filtered and evaporated to give 5-(4-phenoxyphenylmethyl)-1H-tetrazole as a white solid.

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 19 hours
  3. washwashed with diethyl ether (3×50 ml)
  4. washthen washed with 5:1 ethyl acetate/tetrahydrofuran (60 ml) and ethyl acetate (2×50 ml)
  5. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-25fc14e42f424677aa73d3c6c5b9ae9d
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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