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

Sodium hydride → HCID 68325504、化合物

HRID 2403273
ノート
印刷プレビュー

反応式

HRID 2403273 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][CH:10]([C:13]2[CH:18]=[CH:17][C:16]([NH2:19])=[CH:15][CH:14]=2)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].[Br:22][C:23]1[CH:24]=[CH:25][C:26]([CH:29](OS(C(F)(F)F)(=O)=O)[C:30]([F:33])([F:32])[F:31])=[N:27][CH:28]=1>C1COCC1.C(OCC)(=O)C>[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][CH:10]([C:13]2[CH:18]=[CH:17][C:16]([NH:19][CH:29]([C:26]3[CH:25]=[CH:24][C:23]([Br:22])=[CH:28][N:27]=3)[C:30]([F:33])([F:32])[F:31])=[CH:15][CH:14]=2)[CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 24758Sodium hydrideHCID 57365069Tert-butyl 3-(4-aminophenyl)pyrrolidine-1-carboxylateHCID 86664596HCID 86664596、化合物

生成物 1

HCID 68325504HCID 68325504、化合物収率 36%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857
Ethyl Acetate
溶媒

実験手順

To a stirred solution of (RS)-3-(4-amino-phenyl)-pyrrolidine-1-carboxylic acid tert-butyl ester (50 mg, CAS 908334-28-1) in dry THF (0.1 ml) under an argon atmosphere was added sodium hydride (14 mg, 60% dispersion in mineral oil) and stirring was continued for 15 minutes. Trifluoro-methanesulfonic acid 1-(5-bromo-pyridin-2-yl)-2,2,2-trifluoro-ethyl ester (74 mg) was then added and the mixture was stirred overnight at room temperature. The reaction mixture was diluted with ethyl acetate and washed sequentially with water and with saturared brine. The organic phase was separated, dried over sodium sulphate, and concentrated in vacuo. The reside was purified by flash column chromatography (silical gel; gradient: heptane/EtOAc) to give (RS)-3-{4-[(RS)-1-(5-bromo-pyridin-2-yl)-2,2,2-trifluoro-ethylamino]-phenyl}-pyrrolidine-1-carboxylic acid tert-butyl ester (34 mg, 36%) as a yellow oil. MS (ISP): 501.9 ([{81Br}M+H]+), 500.2 ([{79Br}M+H]+), 446.2 ([{81Br}M+H—C4H8]+), 444.1 ([{79Br}M+H—C4H8]+).

後処理

  1. stirringthe mixture was stirred overnight at room temperature
  2. washwashed sequentially with water and with saturared brine
  3. customThe organic phase was separated
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated in vacuo
  6. customThe reside was purified by flash column chromatography (silical gel; gradient: heptane/EtOAc)

出典と根拠

ORDレコード
ord-29bc201d39294dd7a1aeac1022687cb8
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08802673B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート