Hydrochloric Acid → Iptakalim Hydrochloride

HRID 227287노트

반응식

HRID 227287 반응식
[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]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 10057607642407-44-1

생성물 1

HCID 11446679Iptakalim Hydrochloride수율 95.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-933aad5b0f9948f084f4bb379f37a72c
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560473B2

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