ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Carbamate → (3R,4R)-3-(6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)-4-methyl-N-(pyrimidin-4-yl)piperidine-1-carboxamide

HRID 1969636
ノート
印刷プレビュー

反応式

HRID 1969636 の反応式
[C:1](=[O:4])([O-])[NH2:2].Cl.[CH3:6][C@@H:7]1[CH2:12][CH2:11][NH:10][CH2:9][C@@H:8]1[C:13]1[N:17]2[C:18]3[CH:24]=[CH:23][NH:22][C:19]=3[N:20]=[CH:21][C:16]2=[CH:15][N:14]=1.CC[N:27]([CH:31](C)C)[CH:28]([CH3:30])C.C[C:35]#[N:36]>>[C:13]1([C@@H:8]2[C@H:7]([CH3:6])[CH2:12][CH2:11][N:10]([C:1]([NH:2][C:35]3[CH:30]=[CH:28][N:27]=[CH:31][N:36]=3)=[O:4])[CH2:9]2)[N:17]2[C:18]3[CH:24]=[CH:23][NH:22][C:19]=3[N:20]=[CH:21][C:16]2=[CH:15][N:14]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 276CarbamateHCID 6342Acetonitrile2 回HCID 81531DiisopropylethylamineHCID 672171491-((3R,4R)-4-methylpiperidin-3-yl)-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazine hydrochloride

生成物 1

HCID 67999614(3R,4R)-3-(6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)-4-methyl-N-(pyrimidin-4-yl)piperidine-1-carboxamide収率 9%

反応条件

温度
70 °C

実験手順

To solution of 4-aminopyrimidine (0.04 g, 0.43 mmol), TEA (0.07 mL, 0.47 mmol) and DMAP (0.006 g, 0.05 mmol), in MeCN (1 mL) at about 0° C. was added phenyl chloroformate (0.05 mL, 0.41 mmol). The reaction mixture was warmed to ambient temperature and stirred for about 3 h. To the reaction mixture was added water (2 mL) and Et2O (5 mL). The organic layer was separated, washed with water (2 mL), dried over anhydrous MgSO4, filtered, and concd under reduced pressure to provide the crude carbamate. The carbamate was dissolved in MeCN (1 mL) and to it was added a solution of 1-((3R,4R)-4-methylpiperidin-3-yl)-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazine hydrochloride (0.06 g, 0.21 mmol, Example #5 Step J) and DIEA (0.04 mL, 0.21 mmol) in MeCN (1 mL). The reaction mixture was heated to about 70° C. for about 2 h. The solvent was removed under reduced pressure. The crude residue was dissolved in DCM (5 mL) and washed with water (2 mL), brine (3 mL), dried over anhydrous MgSO4, filtered, and concd under reduced pressure. The crude material was purified by RP-HPLC (Table 1, Method e) to give (3R,4R)-3-(6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)-4-methyl-N-(pyrimidin-4-yl)piperidine-1-carboxamide (0.007 g, 9%): LC/MS (Table 1, Method b) Rt=1.40 min; MS m/z 377 (M+H)+.

後処理

  1. customThe solvent was removed under reduced pressure
  2. dissolutionThe crude residue was dissolved in DCM (5 mL)
  3. washwashed with water (2 mL), brine (3 mL)
  4. dry with materialdried over anhydrous MgSO4
  5. filtrationfiltered
  6. customThe crude material was purified by RP-HPLC (Table 1, Method e)

出典と根拠

ORDレコード
ord-2a68e081ac8d4703bec0577e598b2d6d
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08426411B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート