Ammonium Chloride → HCID 178441408, 화합물

HRID 487683노트

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HRID 487683 반응식
[C:1]([C:5]1[N:6]=[C:7]([C:10]2[O:11][C:12]3[CH:18]=[CH:17][C:16]([O:19][CH2:20][C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[CH2:27][C:28]#[N:29])=[CH:15][C:13]=3[CH:14]=2)[S:8][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].[N-:30]=[N+:31]=[N-:32].[Na+].[Cl-].[NH4+]>CN(C)C=O>[C:1]([C:5]1[N:6]=[C:7]([C:10]2[O:11][C:12]3[CH:18]=[CH:17][C:16]([O:19][CH2:20][C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[CH2:27][C:28]4[NH:32][N:31]=[N:30][N:29]=4)=[CH:15][C:13]=3[CH:14]=2)[S:8][CH:9]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 19092790HCID 19092790, 화합물

생성물 1

HCID 178441408HCID 178441408, 화합물수율 47.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
110 °C

실험 절차

A mixture of 4-tert-butyl-2-[5-(2-cyanomethylphenylmethoxy)benzofuran-2-yl]thiazole (0.40 g), sodium azide (0.58 g) and ammonium chloride (0.66 g) in N,N-dimethylformamide (4 ml) was stirred at 110° C. for 8 hours. After being cooled, the mixture was poured into ice-water and extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate and concentrated in reduced pressure to give a syrup. The syrup was subjected to column chromatography on silica gel and eluted with chloroform, successively with a mixture of chloroform and methanol (10:1). The fractions containing object compound were combined and concentrated under reduced pressure to give 5-{2-(2-(4-tert-butylthiazol-2-yl)benzofuran-5-yloxymethyl]phenylmethyl}-1H-tetrazole (0.21 g).

후처리

  1. temperatureAfter being cooled
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in reduced pressure
  6. customto give a syrup
  7. washeluted with chloroform, successively with a mixture of chloroform and methanol (10:1)
  8. additionThe fractions containing object compound
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d34ff6f00adf444da27bdd9895a29bed
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05296495

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