Acetic Acid → (Pyren-1-ylmethylene)malononitrile

HRID 2071220

반응식

HRID 2071220 반응식
[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]

참가 물질

9

반응물 4

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

생성물 1

HCID 290168(Pyren-1-ylmethylene)malononitrile

시약·촉매·용매 4

HCID 241Benzene용매HCID 702Ethanol용매HCID 7964Chlorobenzene용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-594a1e39b8c946db91723e8bd20b0ad2
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04046563

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