Hydrochloric Acid → Iptakalim Hydrochloride

HRID 227287ノート

反応式

HRID 227287 の反応式
[CH3:1][CH:2]([NH:4][C:5]([CH3:10])([CH:7]([CH3:9])[CH3:8])[CH3:6])[CH3:3].[ClH:11]>C(O)C>[CH3:1][CH:2]([NH:4][C:5]([CH3:10])([CH:7]([CH3:9])[CH3:8])[CH3:6])[CH3:3].[ClH:11]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 10057607642407-44-1

生成物 1

HCID 11446679Iptakalim Hydrochloride収率 95.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 100.0 g N-(1-methylethyl)-2,3-dimethyl-2-butylamine in 200 mL ethanol, 100 mL hydrochloric acid was added with shaking and cooling in an glacial water bath. The solvent was distilled off to dry in vacuum. The residue was dissolve in ethanol, then distilled off to dry in vacuum and crystallized from 1:1 i-PrOH-c-Hex-H to give a solid 130.5 g (95.5%), mp 228-230° C.(i-PrOH:Et2O). Elemental analysis for C9H22ClN(%): Calculated C, 60.14; H, 12.34; N, 7.79; Cl, 19.73. Found C, 60.14; H, 12.48; N, 7.31; Cl, 19.67. 1H-NMR (D2O, ppm) 0.98(d, J=6.75H, 6H), 1.33(s, 6H), 1.37(d, J=6.46, 6H), 2.10(m, 1H), 3.70(m, 1H). MS(m/z) 143(M+), 100(B).

後処理

  1. temperaturecooling in an glacial water bath
  2. distillationThe solvent was distilled off
  3. customto dry in vacuum
  4. dissolutionThe residue was dissolve in ethanol
  5. distillationdistilled off
  6. customto dry in vacuum
  7. customcrystallized from 1:1 i-PrOH-c-Hex-H

出典と根拠

ORDレコード
ord-933aad5b0f9948f084f4bb379f37a72c
出典データセット
uspto-grants-2009_07
特許番号
US07560473B2

反応ノート

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