Hydrochloric Acid → (1R)-1-[6-(Trifluoromethyl)(3-pyridyl)]ethylamine

HRID 1842546노트

반응식

HRID 1842546 반응식
CC(S([NH:7][C@@H:8]([C:10]1[CH:11]=[N:12][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:14][CH:15]=1)[CH3:9])=O)(C)C.Cl>CO>[F:18][C:16]([F:17])([F:19])[C:13]1[N:12]=[CH:11][C:10]([C@H:8]([NH2:7])[CH3:9])=[CH:15][CH:14]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 581035742-methyl-N-{(1R)-1-[6-(trifluoromethyl)-3-pyridinyl]ethyl}-2-propanesulfinamide

생성물 1

HCID 55278063(1R)-1-[6-(Trifluoromethyl)(3-pyridyl)]ethylamine수율 98.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 2-methyl-N-{(1R)-1-[6-(trifluoromethyl)-3-pyridinyl]ethyl}-2-propanesulfinamide (41.6 g, 141 mmol) in methyl alcohol (470 mL) at 0° C. was added hydrogen chloride (4.0 M in dioxane; 106 mL, 424 mmol). After 30 min, the mixture was concentrated to dryness. The residue was recrystallized using ethyl alcohol (15 mL) and ether (40 mL). The white solid was filtered and dried under reduced pressure to give the hydrochloride salt of the title compound (26.3 g). MS 191.2 (M+1). 1H NMR (500 MHz, CD3 OD): δ 8.83 (d, J=2.2 Hz, 1 H); 8.17 (d, J=8.2 Hz, 1 H); 7.93 (d, J=8.2 Hz, 1 H); 4.69 (q, J=6.9 Hz, 1 H); 1.70 (d, J=6.9 Hz, 3 H).

후처리

  1. concentrationthe mixture was concentrated to dryness
  2. customThe residue was recrystallized
  3. filtrationThe white solid was filtered
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-e7a054ecf03348edad327bf9fbff9c3e
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946231B2

반응 노트

불러오는 중…