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Ammonia → HCID 68424460、化合物

HRID 1984993
ノート
印刷プレビュー

反応式

HRID 1984993 の反応式
O.Cl.O[C:4]1([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:8][CH2:7][C:6]([C:9]2[CH:10]=[CH:11][CH:12]=[C:13]3[C:18]=2[N:17]=[CH:16][CH:15]=[CH:14]3)=[C:5]1[CH3:19].N>O1CCCC1>[CH3:19][C:5]1[C:4]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[CH:8][CH2:7][C:6]=1[C:9]1[CH:10]=[CH:11][CH:12]=[C:13]2[C:18]=1[N:17]=[CH:16][CH:15]=[CH:14]2
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 962WaterHCID 68425885HCID 68425885、化合物

生成物 1

HCID 68424460HCID 68424460、化合物収率 69.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 5 ml of water and 5 ml of concentrated hydrochloric acid was added to a solution of 1.717 g (5.7 mmol) of 3-hydroxy-2-methyl-3-phenyl-1-(8-quinolyl)cyclopentene in 100 ml of tetrahydrofuran. The mixture was stirred at room temperature for 90 minutes and ammonia solution was then added until a pH of 12 had been reached. The aqueous phase was then separated off from the organic phase and the aqueous phase was extracted twice with diethyl ether. The organic phases were combined, dried over magnesium sulfate, filtered and the solvent was distilled off. The residue obtained in this way was distilled at 157-170° C. and 2×10−2 mbar to give 1.12 g (3.95 mmol, 69.3%) of 2-methyl-3-phenyl-1-(8-quinolyl)cyclopentadiene.

後処理

  1. customThe aqueous phase was then separated off from the organic phase
  2. extractionthe aqueous phase was extracted twice with diethyl ether
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. distillationthe solvent was distilled off
  6. customThe residue obtained in this way
  7. distillationwas distilled at 157-170° C.

出典と根拠

ORDレコード
ord-3c7a7b7f6a2e4eef91fa3203cd28cf2c
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07544826B2

反応ノート

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