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Ammonia → HCID 18968908, 화합물

HRID 398790
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HRID 398790 반응식
Cl.[NH2:2][CH:3]1[C:9](=[O:10])[NH:8][C:7]2[CH:11]=[CH:12][C:13]3[C:18]([C:6]=2[CH2:5][CH2:4]1)=[CH:17][CH:16]=[CH:15][CH:14]=3.N>O>[NH2:2][CH:3]1[C:9](=[O:10])[NH:8][C:7]2[CH:11]=[CH:12][C:13]3[C:18]([C:6]=2[CH2:5][CH2:4]1)=[CH:17][CH:16]=[CH:15][CH:14]=3
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참가 물질

4

반응물 2

HCID 222AmmoniaHCID 18968915HCID 18968915, 화합물

생성물 1

HCID 18968908HCID 18968908, 화합물수율 97.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of 3-azido-4-oxo-2,3,4,5-tetrahydro-1H-naphtho-[2,1-b]azepine (16.0 g, 63.4 mmol) in a mixture of dry dioxane (150 ml) and ethanol (150 ml), palladium on carbon (10%, 2 g) was added. This mixture was hydrogenated under a pressure of 5 bar and with efficient stirring for 24 h. The reaction mixture was filtered and excess hydrogenchloride in ethanol was added. The precipitated solid was isolated, washed with ethanol and dried to give 14.4 g of 3-amino-4-oxo-2,3,4,5-tetrahydro-1H-naphtho[2,1-b]azepine hydrochloride. The above hydrochloride (14.2 g) was dissolved into water (800 ml) by warming. A 25% aqueous ammonia solution was added and a precipitate was formed. The solid was isolated by filtration, washed with water and dried in vacuo to give 11.9 g of 3-amino-4-oxo-2,3,4,5-tetrahydro-1H-naphtho[2,1-b]azepine.

후처리

  1. temperatureby warming
  2. customa precipitate was formed
  3. customThe solid was isolated by filtration
  4. washwashed with water
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-e1b24c1230fa4921b11737de325bd374
출처 데이터셋
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05817654

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