Tetrahydrofuran → HCID 178515336、化合物

HRID 1075025ノート

反応式

HRID 1075025 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 178515336HCID 178515336、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-75ae7bdc15cd4bd8b5ef778be119a9a4
出典データセット
uspto-grants-1983_07
特許番号
US04394515

反応ノート

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