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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
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Triethylamine → HCID 66841547、化合物

HRID 2267707
ノート
印刷プレビュー

反応式

HRID 2267707 の反応式
O[C@H:2](C)[CH2:3][N:4]1[CH2:9][CH2:8][CH:7]([O:10][C:11](=[O:16])[C:12]([CH3:15])([CH3:14])[CH3:13])[CH2:6][CH2:5]1.[CH2:18]([N:20]([CH2:23][CH3:24])[CH2:21][CH3:22])C.S(OS(C(F)(F)F)(=O)=O)(C(F)(F)F)(=O)=O.[C:40]([O:44][C:45](=[O:53])[NH:46][CH:47]1CCNCC1)([CH3:43])([CH3:42])[CH3:41]>C(Cl)Cl>[C:40]([O:44][C:45]([NH:46][CH:47]1[CH2:24][CH2:23][N:20]([CH2:18][C@@H:3]([N:4]2[CH2:5][CH2:6][CH:7]([O:10][C:11](=[O:16])[C:12]([CH3:13])([CH3:14])[CH3:15])[CH2:8][CH2:9]2)[CH3:2])[CH2:21][CH2:22]1)=[O:53])([CH3:43])([CH3:42])[CH3:41]
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 4

HCID 8471TriethylamineHCID 67749Trifluoromethanesulfonic anhydrideHCID 7238334-(N-Boc-amino)piperidineHCID 675236702,2-Dimethyl-propionic acid 1-((R)-2-hydroxy-propyl)-piperidin-4-yl ester

生成物 1

HCID 66841547HCID 66841547、化合物

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

実験手順

A solution of alcohol 53 (1.26 g, 5.16 mmol) and triethylamine (1.43 ml, 10.32 mmol) in 80 ml of DCM is cooled to −78 C. Triflic anhydride (0.85 ml, 5.16 mmol) is slowly added and stirring continued for 1 hour. The mixture is then allowed to warm up to 0 C and cooled back to −78 C after 15 minutes. A solution of piperidin-4-yl-carbamic acid tert-butyl ester, 3, (1.03 g, 5.16 mmol) in 40 ml of DCM is slowly added at −78 C. After complete addition, the cooling bath is removed and the dark solution is allowed to warm up to room temperature. The mixture is washed twice with water, dried over sodium sulphate, filtered and evaporated. The crude is purified by chromatography on silicagel using DCM (saturated with ammonia) and MeOH (1%).

後処理

  1. temperatureto warm up to 0 C
  2. temperaturecooled back to −78 C after 15 minutes
  3. additionAfter complete addition
  4. customthe cooling bath is removed
  5. washThe mixture is washed twice with water
  6. dry with materialdried over sodium sulphate
  7. filtrationfiltered
  8. customevaporated
  9. customThe crude is purified by chromatography on silicagel

出典と根拠

ORDレコード
ord-8607e86cdb2f4ae383dd0f694846a961
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07858781B2

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