Hydrochloric Acid → 1-[6-(1,1-Difluoro-butyl)-3,3-dimethyl-2,3-dihydro-pyrrolo[3,2-b]pyridin-1-yl]-2-[(2R,5R)-5-methyl-2-((R)-3-methyl-morpholin-4-ylmethyl)-piperazin-1-yl]-ethanone dihydrochloride

HRID 1475527노트

반응식

HRID 1475527 반응식
[ClH:1].C(OC([N:9]1[CH2:14][C@H:13]([CH2:15][N:16]2[CH2:21][CH2:20][O:19][CH2:18][C@H:17]2[CH3:22])[N:12]([CH2:23][C:24]([N:26]2[C:34]3[C:29](=[N:30][CH:31]=[C:32]([C:35]([F:40])([F:39])[CH2:36][CH2:37][CH3:38])[CH:33]=3)[C:28]([CH3:42])([CH3:41])[CH2:27]2)=[O:25])[CH2:11][C@H:10]1[CH3:43])=O)(C)(C)C>O1CCOCC1.CCOC(C)=O>[ClH:1].[ClH:1].[F:39][C:35]([C:32]1[CH:33]=[C:34]2[N:26]([C:24](=[O:25])[CH2:23][N:12]3[CH2:11][C@@H:10]([CH3:43])[NH:9][CH2:14][C@@H:13]3[CH2:15][N:16]3[CH2:21][CH2:20][O:19][CH2:18][C@H:17]3[CH3:22])[CH2:27][C:28]([CH3:42])([CH3:41])[C:29]2=[N:30][CH:31]=1)([F:40])[CH2:36][CH2:37][CH3:38]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 70981092(2R,5S)-4-{2-[6-(1,1-Difluoro-butyl)-3,3-dimethyl-2,3-dihydro-pyrrolo[3,2-b]pyridin-1-yl]-2-oxo-ethyl}-2-methyl-5-((R)-3-methyl-morpholin-4-ylmethyl)-piperazine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 714718871-[6-(1,1-Difluoro-butyl)-3,3-dimethyl-2,3-dihydro-pyrrolo[3,2-b]pyridin-1-yl]-2-[(2R,5R)-5-methyl-2-((R)-3-methyl-morpholin-4-ylmethyl)-piperazin-1-yl]-ethanone dihydrochloride

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

4N HCl in dioxane (35 mL) was added to a solution of (2R,5S)-4-{2-[6-(1,1-difluoro-butyl)-3,3-dimethyl-2,3-dihydro-pyrrolo[3,2-b]pyridin-1-yl]-2-oxo-ethyl}-2-methyl-5-((R)-3-methyl-morpholin-4-ylmethyl)-piperazine-1-carboxylic acid tert-butyl ester (2.1 g) in EtOAc (10 mL). The resulting suspension was stirred for 1 h at room temperature. The solvent was then removed in vacuo. The solid was triturated in Et2O, collected by filtration, washed with Et2O and dried in vacuo to give the title compound (1.7 g) as a yellow solid. 1H NMR (Me-d3-OD): 8.77 (1H, s), 8.52 (1H, s), 4.36-3.91 (9H, m), 3.91-3.41 (8H, m), 3.18-2.99 (1H, m), 2.34-2.15 (2H, m), 1.67-1.36 (15H, m), 1.00 (3H, t). MS: [M+H]+=494.

후처리

  1. customThe solvent was then removed in vacuo
  2. customThe solid was triturated in Et2O
  3. filtrationcollected by filtration
  4. washwashed with Et2O
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-2fc7fab0e4f049989f15924abb26c7f3
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09018214B2

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