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

HCID 117966280、化合物 → HCID 117966443、化合物

HRID 931098
ノート
印刷プレビュー

反応式

HRID 931098 の反応式
[CH2:1]1[N:5]=[C:4]([CH:6]2[CH2:11][CH2:10][CH2:9][N:8]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:7]2)[N:3]2[CH2:19][CH2:20][CH2:21][CH:2]12>C1(C)C=CC=CC=1>[CH:1]1[N:5]=[C:4]([CH:6]2[CH2:11][CH2:10][CH2:9][N:8]([C:12]([O:14][C:15]([CH3:18])([CH3:16])[CH3:17])=[O:13])[CH2:7]2)[N:3]2[CH2:19][CH2:20][CH2:21][C:2]=12
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

3

反応物 1

HCID 117966280HCID 117966280、化合物

生成物 1

HCID 117966443HCID 117966443、化合物収率 14.3%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
115 °C

実験手順

To a solution of tert-butyl 3-(5,6,7,7a-tetrahydro-1H-pyrrolo[1,2-c]imidazol-3-yl)piperidine-1-carboxylate (175 mg, 0.6 mmol) in toluene (5 mL) was added BaMnO4 (2.1 g, 18 mmol) and the reaction was heated at 115° C. for 42 h. The reaction was cooled to room temperature and BaMnO4 (2 g) was added followed by toluene (2 mL). The reaction mixture was heated to 115° C. for 3 days. The mixture was cooled to room temperature and filtered through Celite followed by rinsing with dichloromethane. The filtrate was concentrated under reduced pressure and the residue was purified via HPLC to afford tert-butyl 3-(6,7-dihydro-5H-pyrrolo[1,2-c]imidazol-3-yl)piperidine-1-carboxylate as an oil (25 mg, 14%). MS (ES+) (M+H) 292.2; LCMS retention time: 1.69 minutes (Method M).

後処理

  1. temperatureThe reaction was cooled to room temperature
  2. temperatureThe reaction mixture was heated to 115° C. for 3 days
  3. temperatureThe mixture was cooled to room temperature
  4. filtrationfiltered through Celite
  5. washby rinsing with dichloromethane
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. customthe residue was purified via HPLC

出典と根拠

ORDレコード
ord-7990401f3b1a418cae8ba944866afb0a
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09296745B2

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