Ammonia → HCID 13672845, 화합물

HRID 652408노트

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HRID 652408 반응식
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

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 20197205HCID 20197205, 화합물

생성물 1

HCID 13672845HCID 13672845, 화합물수율 99.2%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a1f5bb520c584909b7279a90d19434ed
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04672062

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