Formaldehyde → HCID 12928524、化合物

HRID 1632679ノート

反応式

HRID 1632679 の反応式
[Cl:1][C:2]1[C:18]([O:19][CH3:20])=[CH:17][C:5]2[C@H:6]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH2:7][NH:8][CH2:9][CH2:10][C:4]=2[CH:3]=1.[CH2:21]=O>C(O)=O>[Cl:1][C:2]1[C:18]([O:19][CH3:20])=[CH:17][C:5]2[C@H:6]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH2:7][N:8]([CH3:21])[CH2:9][CH2:10][C:4]=2[CH:3]=1

参加物

4

反応物 2

HCID 712FormaldehydeHCID 12928521HCID 12928521、化合物

生成物 1

HCID 12928524HCID 12928524、化合物

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

Reflux for 4 hours, a solution of 52.0 g (0.18 moles) of the product of step C in a mixture of 96 ml of 37% formaldehyde and 144 ml of 90% formic acid. Distill almost to dryness at 100° C. under reduced pressure (about 100 mm). Dissolve the residue in a mixture of 500 ml of 1 N sodium hydroxide and 500 ml of ethyl ether with cooling and stirring. Separate the ether layer, dry over anhydrous sodium sulfate, and evaporate to give (S)-7-chloro-8-methoxy-3-methyl-1-phenyl-2,3,4,5- tetrahydro-1H-3-benzazepine as a colorless solid. Obtain an analytically pure sample by crystallization from ethyl ether, m.p. 91°-92° C., [α]D26 =+47.3°(c=1, ethanol).

後処理

  1. temperatureReflux for 4 hours
  2. distillationDistill almost to dryness at 100° C. under reduced pressure (about 100 mm)
  3. dissolutionDissolve the residue
  4. additionin a mixture of 500 ml of 1 N sodium hydroxide and 500 ml of ethyl ether
  5. temperaturewith cooling
  6. customSeparate the ether layer
  7. dry with materialdry over anhydrous sodium sulfate
  8. customevaporate

出典と根拠

ORDレコード
ord-13e2d76d0d01460cad289300a181305a
出典データセット
uspto-grants-1984_10
特許番号
US04477378

反応ノート

読み込み中…