2,5-Dimethoxytetrahydrofuran → HCID 14986610、化合物

HRID 373870ノート

反応式

HRID 373870 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[CH2:11][CH2:10][N:9]([CH:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:8][CH2:7]1.CO[CH:27]1[CH2:31][CH2:30][CH:29](OC)O1>C(O)(=O)C>[C:13]1([CH:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[N:9]2[CH2:10][CH2:11][N:6]([CH2:5][CH2:4][CH2:3][CH2:2][N:1]3[CH:27]=[CH:31][CH:30]=[CH:29]3)[CH2:7][CH2:8]2)[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

参加物

4

反応物 2

HCID 790982,5-DimethoxytetrahydrofuranHCID 139569931-(4-Aminobutyl)-4-(diphenylmethyl)piperazine

生成物 1

HCID 14986610HCID 14986610、化合物収率 64.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Under reflux, for 20 minutes is heated a solution of 1.28 g (3.96 mmoles) of 1-(4-aminobutyl)-4-diphenylmethylpiperazine and 0.77 g (5.8 mmoles) of 2.5-dimethoxytetrahydrofurane in 25 ml of acetic acid. It is cooled, it is poured over ice water, neutralized with NaCHO3 and extracted with chloroform. It is dried with Na2SO4, and evaporated under vacuum to dryness. 1.7 g of crude oil is obtained which is purified on a silica chromatographic column (eluant: ethyl acetate). 0.95 g of 1-[4-(4-Diphenylmethyl-1-piperazinyl)butyl]pyrrole is obtained in solid form, with a melting point 80°-84° C.

後処理

  1. temperatureUnder reflux, for 20 minutes
  2. temperatureIt is cooled
  3. extractionextracted with chloroform
  4. dry with materialIt is dried with Na2SO4
  5. customevaporated under vacuum to dryness
  6. custom1.7 g of crude oil is obtained which
  7. customis purified on a silica chromatographic column (eluant: ethyl acetate)

出典と根拠

ORDレコード
ord-01eb4e09f7ec46e6914686cb10c101cc
出典データセット
uspto-grants-1992_11
特許番号
US05166205

反応ノート

読み込み中…