Acetic Acid → (Pyren-1-ylmethylene)malononitrile

HRID 2071220

反応式

HRID 2071220 の反応式
[C:1]1([CH:17]=O)[C:14]2[C:15]3=[C:16]4[C:11](=[CH:12][CH:13]=2)[CH:10]=[CH:9][CH:8]=[C:7]4[CH:6]=[CH:5][C:4]3=[CH:3][CH:2]=1.[C:19](#[N:23])[CH2:20][C:21]#[N:22].C(O)(=O)C.C([O-])(=O)C.[NH4+]>C(O)C.ClC1C=CC=CC=1.O1CCCC1.C1C=CC=CC=1>[C:21]([C:20]([C:19]#[N:23])=[CH:17][C:1]1[C:14]2[C:15]3=[C:16]4[C:11](=[CH:12][CH:13]=2)[CH:10]=[CH:9][CH:8]=[C:7]4[CH:6]=[CH:5][C:4]3=[CH:3][CH:2]=1)#[N:22]

参加物

9

反応物 4

HCID 176Acetic AcidHCID 8010MalononitrileHCID 2328481-PyrenecarboxaldehydeHCID 517165Ammonium Acetate

生成物 1

HCID 290168(Pyren-1-ylmethylene)malononitrile

試薬・触媒・溶媒 4

HCID 241Benzene溶媒HCID 702Ethanol溶媒HCID 7964Chlorobenzene溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

About 100 grams (0.434 moles) pyrene-1-carboxaldehyde, about 28.7 grams (0.434 moles) malononitrile, about 10.4 milliliters acetic acid, about 3.48 grams ammonium acetate and about 400 milliliters benzene are heated to boiling under reflux conditions for 30 minutes. The entire contents of the flask crystallized, forming a deep orange red product which is soluble in -tetrahydrofuran, moderately soluble in ethanol and very soluble in chlorobenzene. This product is recrystallized from a mixture of chlorobenzene and ethanol (30:70). Yield: 104.4 grams m. p 248°-250° C.

後処理

  1. customThe entire contents of the flask crystallized
  2. customforming a deep orange red product which
  3. customThis product is recrystallized from a mixture of chlorobenzene and ethanol (30:70)
  4. customp 248°-250° C.

出典と根拠

ORDレコード
ord-594a1e39b8c946db91723e8bd20b0ad2
出典データセット
uspto-grants-1977_09
特許番号
US04046563

関連ノート

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