5-Bromo-1-methyl-1H-tetrazole → HCID 20403203、化合物

HRID 2164744ノート

反応式

HRID 2164744 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 20403203HCID 20403203、化合物収率 55.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-68a4605673704cfebaac9762fb2aff03
出典データセット
uspto-grants-1985_03
特許番号
US04507296

反応ノート

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