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Potassium Hydroxide → 5,6-dihydro-2-[4-[3-(4-piperidinyl)propoxy]phenyl]-4H-1,3-oxazine

HRID 484492
ノート
印刷プレビュー

反応式

HRID 484492 の反応式
[O:1]1[CH2:6][CH2:5][CH2:4][N:3]=[C:2]1[C:7]1[CH:27]=[CH:26][C:10]([O:11][CH2:12][CH2:13][CH2:14][CH:15]2[CH2:20][CH2:19][N:18](C(OCC)=O)[CH2:17][CH2:16]2)=[CH:9][CH:8]=1.[OH-].[K+]>CC(O)C>[NH:18]1[CH2:19][CH2:20][CH:15]([CH2:14][CH2:13][CH2:12][O:11][C:10]2[CH:26]=[CH:27][C:7]([C:2]3[O:1][CH2:6][CH2:5][CH2:4][N:3]=3)=[CH:8][CH:9]=2)[CH2:16][CH2:17]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 14989203ethyl 4-[3-[4-(5,6-dihydro-4H-1,3-oxazin-2-yl)phenoxy]propyl]-1-piperidinecarboxylate

生成物 1

HCID 149892045,6-dihydro-2-[4-[3-(4-piperidinyl)propoxy]phenyl]-4H-1,3-oxazine収率 100%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of ethyl 4-[3-[4-(5,6-dihydro-4H-1,3-oxazin-2-yl)phenoxy]propyl]-1-piperidinecarboxylate, 26,3 parts of potassium hydroxide and 200 parts of 2-propanol was stirred and refluxed for 3 hours. After evaporation, water was added ant eh solvent was distilled off till all traces of 2-propanol were removed. After cooling, ice water was added to the product was extracted with dichloromethane. The organic layer was dried, filtered and evaporated, yielding 14.5 parts (100%) of 5,6-dihydro-2-[4-[3-(4-piperidinyl) propoxy]phenyl]-4H-1,3-oxazine as a residue (int. 60).

後処理

  1. temperaturerefluxed for 3 hours
  2. customAfter evaporation, water
  3. additionwas added ant eh solvent
  4. distillationwas distilled off till all traces of 2-propanol
  5. customwere removed
  6. temperatureAfter cooling
  7. additionice water was added to the product
  8. extractionwas extracted with dichloromethane
  9. customThe organic layer was dried
  10. filtrationfiltered
  11. customevaporated

出典と根拠

ORDレコード
ord-abdcf5f7227f4524bf2811fd04bf8578
出典データセット
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05231184

反応ノート

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