Hydrochloric Acid → Isopropanol

HRID 2267192노트

반응식

HRID 2267192 반응식
[CH:1]1([CH2:4][N:5]([C:13]2[C:14]([CH2:23][CH3:24])=[N:15][N:16]3[C:21]([I:22])=[CH:20][CH:19]=[CH:18][C:17]=23)[CH2:6][CH:7]2[CH2:12][CH2:11][O:10][CH2:9][CH2:8]2)[CH2:3][CH2:2]1.[ClH:25].C(=O)(OC)[O:27]C>C(O)(C)C>[ClH:25].[CH:1]1([CH2:4][N:5]([C:13]2[C:14]([CH2:23][CH3:24])=[N:15][N:16]3[C:21]([I:22])=[CH:20][CH:19]=[CH:18][C:17]=23)[CH2:6][CH:7]2[CH2:12][CH2:11][O:10][CH2:9][CH2:8]2)[CH2:3][CH2:2]1.[CH:12]([OH:27])([CH3:11])[CH3:7]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 12021Dimethyl Carbonate3회HCID 11339625N-Cyclopropylmethyl-2-ethyl-7-iodo-N-(tetrahydro-2H-pyran-4-ylmethyl)pyrazolo[1,5-a]pyridine-3-amine

생성물 2

HCID 3776Isopropanol수율 93.7%HCID 21084143N-Cyclopropylmethyl-N-(2-ethyl-7-iodopyrazolo[1,5-a]pyridin-3-yl)-N-tetrahydro-2H-4-pyranylmethylamine hydrochloride

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

Into a solution of N-cyclopropylmethyl-N-(2-ethyl-7-iodopyrazolo[1,5-a]pyridin e-3-yl)-N-(tetrahydro-2H-4-pyranylmethyl)amine (220 g, 501 mmol) in dimethyl carbonate (3600 mL) was dropped a solution of concentrated hydrochloric acid (48.5 mL, 575 mmol) in isopropanol (270 mL) at room temperature over a period of 20 minutes, and the mixture was further stirred at room temperature for about 15 hours. The reaction mixture was cooled in an ice water bath, and to the reaction mixture was added dimethyl carbonate (900 mL). This mixture was stirred for about 5 hours, and a precipitate was filtrated. The precipitate was washed with dimethyl carbonate (900 mL), and dried at 50° C. under reduced pressure, to obtain 250 g of a title compound as a solvate in dimethyl carbonate and isopropanol (yield: 93.7%).

후처리

  1. temperatureThe reaction mixture was cooled in an ice water bath
  2. stirringThis mixture was stirred for about 5 hours
  3. filtrationa precipitate was filtrated
  4. washThe precipitate was washed with dimethyl carbonate (900 mL)
  5. customdried at 50° C. under reduced pressure

출처 및 근거

ORD 기록
ord-7596db0fae704709a2e2478791fc24bd
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07858809B2

반응 노트

불러오는 중…