Ammonia → HCID 13672845、化合物

HRID 652408ノート

反応式

HRID 652408 の反応式
Cl.[CH3:2][NH:3][CH:4]1[CH2:10][CH:9](O)[C:8]2[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=2[O:6][CH2:5]1.N>Cl>[CH3:2][NH:3][CH:4]1[CH:10]=[CH:9][C:8]2[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=2[O:6][CH2:5]1

参加物

4

反応物 2

HCID 222AmmoniaHCID 20197205HCID 20197205、化合物

生成物 1

HCID 13672845HCID 13672845、化合物収率 99.2%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

23.0 g of 3-methylamino-2,3,4,5-tetrahydro-1-benzoxepin-5-ol hydrochloride were heated to 100 degrees C. for 30 minutes with stirring in 50 ml of 32 percent aqueous hydrochloric acid solution. Subsequently, the solution was poured over 100 g of ice, and the mixture was rendered alkaline with 70 ml of 25 percent aqueous ammonia solution. The mixture was thereafter extracted once with 100 ml and four times with 25 ml portions of methylene chloride. The combined methylene chloride extracts were dried over sodium sulfate, and the solvent was distilled off under reduced pressure. 17.4 g of 3-methylamino-2,3-dihydro-1-benzoxepine were obtained as a colorless oil.

後処理

  1. extractionThe mixture was thereafter extracted once with 100 ml and four times with 25 ml portions of methylene chloride
  2. dry with materialThe combined methylene chloride extracts were dried over sodium sulfate
  3. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-a1f5bb520c584909b7279a90d19434ed
出典データセット
uspto-grants-1987_06
特許番号
US04672062

反応ノート

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