Sodium Hydroxide → HCID 178418490, 화합물

HRID 1629

반응식

HRID 1629 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 178418490HCID 178418490, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-25fc14e42f424677aa73d3c6c5b9ae9d
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05726195

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