Methanol → tert-Butyl 6-bromo-4-oxospiro[chroman-2,4'-piperidine]-1'-carboxylate

HRID 38473

反応式

HRID 38473 の反応式
[CH3:1][C:2]([C:4]1[CH:9]=[C:8]([Br:10])[CH:7]=[CH:6][C:5]=1[OH:11])=[O:3].[C:12]([N:19]1[CH2:24][CH2:23][C:22](=O)[CH2:21][CH2:20]1)([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13].N1CCCC1.CO>O>[Br:10][C:8]1[CH:9]=[C:4]2[C:5](=[CH:6][CH:7]=1)[O:11][C:22]1([CH2:23][CH2:24][N:19]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:20][CH2:21]1)[CH2:1][C:2]2=[O:3]

参加物

6

反応物 4

HCID 887MethanolHCID 31268PyrrolidineHCID 959915'-Bromo-2'-hydroxyacetophenoneHCID 735900tert-Butyl 4-oxopiperidine-1-carboxylate

生成物 1

HCID 2794759tert-Butyl 6-bromo-4-oxospiro[chroman-2,4'-piperidine]-1'-carboxylate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 5-bromo-2-hydroxyacetophenone (104 g, 485 mmol), N-Boc-piperidin-4-one (98.6 g, 494 mmol), 20 mL of pyrrolidine (17.3 g, 243 mmol) and 261 mL of MeOH was heated under reflux until the reaction was complete. The mixture was cooled, then 87 mL of H2O were added, and the mixture was filtered and dried to give intended compound as a colorless solid.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux until the reaction
  3. temperatureThe mixture was cooled
  4. filtrationthe mixture was filtered
  5. customdried
  6. customto give

出典と根拠

ORDレコード
ord-de58866a73cb48c7a016ae38f2f5ffeb
出典データセット
uspto-grants-2013_09
特許番号
US08524730B2

関連ノート

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