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11-Chloro-6,11-dihydrodibenz[b,e]oxepin → HCID 12962149, 화합물

HRID 1156276
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HRID 1156276 반응식
Cl[CH:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][CH:15]=[CH:16][C:3]1=2.[C:17]([Cu])#[N:18]>C1C=CC=CC=1>[C:17]([CH:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][CH:15]=[CH:16][C:3]1=2)#[N:18]
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참가 물질

4

반응물 2

HCID 1296214811-Chloro-6,11-dihydrodibenz[b,e]oxepinHCID 178418546HCID 178418546, 화합물

생성물 1

HCID 12962149HCID 12962149, 화합물수율 92%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

11-Chloro-6,11-dihydrodibenz[b,e]oxepin (32.69 g; 0.14 mole) is dissolved in dry benzene (300 ml) and placed under a dry nitrogen atmosphere. To this solution is added in one portion, CuCN (32.04 g; 0.35 mole). The reaction is heated to reflux for 31/2 hours and filtered while hot. After washing the salts with benzene, the filtrate is removed in vacuo to give a solid. This solid is triturated several times with isopropyl ether and finally hexane to give a solid (92%) of 11-cyano-6,11-dihydrodibenz[b,e]oxepin m.p. 65°-66.5° C.

후처리

  1. temperatureThe reaction is heated
  2. temperatureto reflux for 31/2 hours
  3. filtrationfiltered while hot
  4. washAfter washing the salts with benzene
  5. customthe filtrate is removed in vacuo
  6. customto give a solid
  7. customThis solid is triturated several times with isopropyl ether and finally hexane

출처 및 근거

ORD 기록
ord-561e7c14108a4d719f96242573b9a7d0
출처 데이터셋
uspto-grants-1982_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04335122

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