5-Bromo-1-methyl-1H-tetrazole → HCID 20403203, 화합물

HRID 2164744노트

반응식

HRID 2164744 반응식
[NH2:1][CH2:2][CH:3]([OH:20])[CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([CH2:13][N:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[CH:8]=1.Br[C:22]1[N:26]([CH3:27])[N:25]=[N:24][N:23]=1>C(O)C>[CH3:27][N:26]1[C:22]([NH:1][CH2:2][CH:3]([OH:20])[CH2:4][CH2:5][O:6][C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([CH2:13][N:14]3[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]3)[CH:8]=2)=[N:23][N:24]=[N:25]1

참가 물질

4

반응물 2

HCID 127974465-Bromo-1-methyl-1H-tetrazoleHCID 202460151-Amino-4-{3-[(piperidin-1-yl)methyl]phenoxy}butan-2-ol

생성물 1

HCID 20403203HCID 20403203, 화합물수율 55.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 1-amino-4-[3-(1-piperidinylmethyl)phenoxy]-2-butanol (1.39 g) and 5-bromo-1-methyl-1H-tetrazole (0.82 g) in absolute ethanol (10 ml) was heated in an autoclave at 125° for 18 h. The solution was evaporated and the residue dissolved in 1M hydrochloric acid (25 ml). The acidic solution was washed with ethyl acetate, basified with excess sodium carbonate and extracted with ethyl acetate. The extract was dried and evaporated to leave a solid which was triturated with dry diethyl ether to give a white solid (1.0 g). This solid was recrystallised from methyl acetate-light petroleum (b.p. 60°-80°) to give the title compound (0.6 g) as white crystals, m.p. 138°-9°.

후처리

  1. customThe solution was evaporated
  2. dissolutionthe residue dissolved in 1M hydrochloric acid (25 ml)
  3. washThe acidic solution was washed with ethyl acetate
  4. extractionextracted with ethyl acetate
  5. customThe extract was dried
  6. customevaporated
  7. customto leave a solid which
  8. customwas triturated with dry diethyl ether

출처 및 근거

ORD 기록
ord-68a4605673704cfebaac9762fb2aff03
출처 데이터셋
uspto-grants-1985_03
특허 번호
US04507296

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