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 1475527ノート

反応式

HRID 1475527 の反応式
[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]

参加物

5

反応物 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

生成物 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

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2fc7fab0e4f049989f15924abb26c7f3
出典データセット
uspto-grants-2015_04
特許番号
US09018214B2

反応ノート

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