Formaldehyde → Sch-12679

HRID 972348ノート

反応式

HRID 972348 の反応式
[CH3:1][O:2][C:3]1[C:19]([O:20][CH3:21])=[CH:18][C:6]2[CH:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:8][NH:9][CH2:10][CH2:11][C:5]=2[CH:4]=1.[CH2:22]=O>C(O)=O>[CH3:1][O:2][C:3]1[C:19]([O:20][CH3:21])=[CH:18][C:6]2[CH:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:8][N:9]([CH3:22])[CH2:10][CH2:11][C:5]=2[CH:4]=1

参加物

4

反応物 2

HCID 712FormaldehydeHCID 105409631H-3-Benzazepine, 2,3,4,5-tetrahydro-7,8-dimethoxy-1-phenyl-

生成物 1

HCID 5024Sch-12679

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

A solution of 3.58 g. (0.0126 mol) of 7,8-dimethoxy-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine in 15 ml. of formic acid and 10 ml. of formaldehyde is refluxed for 18 hours. The reaction mixture is evaporated to dryness, 20 ml. of 6N hydrochloric acid is added and the solution is again evaporated to dryness to give a liquid. The latter is treated with 20 ml. of 10% sodium hydroxide solution and the mixture is extracted with ether. The dried extract is evaporated to give the liquid 7,8-dimethoxy-3-methyl-1-phenyl-2,3,4,5- tetrahydro-1H-3-benzazepine.

後処理

  1. customThe reaction mixture is evaporated to dryness, 20 ml
  2. additionof 6N hydrochloric acid is added
  3. customthe solution is again evaporated to dryness
  4. customto give a liquid
  5. additionThe latter is treated with 20 ml
  6. extractionof 10% sodium hydroxide solution and the mixture is extracted with ether
  7. extractionThe dried extract
  8. customis evaporated

出典と根拠

ORDレコード
ord-97c0d6969e624b6d9ab17a7b0eca9b6c
出典データセット
uspto-grants-1977_10
特許番号
US04052506

反応ノート

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