Tetrahydrofuran → HCID 178515336, 화합물

HRID 1075025노트

반응식

HRID 1075025 반응식
O1CCCC1.[Cl-].[Al+3].[Cl-].[Cl-].[C:10]([CH2:12][C:13]1[CH:14]=[CH:15][C:16]2[C:22](=[O:23])[CH2:21][C:20]3[CH:24]=[CH:25][CH:26]=[CH:27][C:19]=3[S:18][C:17]=2[CH:28]=1)#[N:11].[N-:29]=[N+:30]=[N-:31].[Na+]>O>[NH:29]1[C:10]([CH2:12][C:13]2[CH:14]=[CH:15][C:16]3[C:22](=[O:23])[CH2:21][C:20]4[CH:24]=[CH:25][CH:26]=[CH:27][C:19]=4[S:18][C:17]=3[CH:28]=2)=[N:11][N:31]=[N:30]1

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 33557Sodium AzideHCID 6451240Aluminum(III) ChlorideHCID 202702303-Cyanomethyl-10,11-dihydro-11-oxodibenzo[b,f]thiepin

생성물 1

HCID 178515336HCID 178515336, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Add to 25 cc. of tetrahydrofuran cooled in an ice bath 1.59 gm. (11.9 mmole) of aluminum chloride, 1.33 gm. (5.25 mmole) of 3-cyanomethyl-10,11-dihydro-11-oxodibenzo[b,f]thiepin and 1.55 gm. (23.8 mmole) of sodium azide. Reflux the mixture for 19 hours, cool, dilute with water and acidify. Extract the mixture into ethyl acetate and evaporate. Triturate the residue in ether and separate the title product by filtration.

후처리

  1. additionAdd to 25 cc
  2. temperatureReflux the mixture for 19 hours
  3. temperaturecool
  4. extractionExtract the mixture into ethyl acetate
  5. customevaporate
  6. customTriturate the residue in ether
  7. customseparate the title product
  8. filtrationby filtration

출처 및 근거

ORD 기록
ord-75ae7bdc15cd4bd8b5ef778be119a9a4
출처 데이터셋
uspto-grants-1983_07
특허 번호
US04394515

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