2-Tridecanone → 2,3-Dihydroperimidine

HRID 1768898

반응식

HRID 1768898 반응식
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[NH2:12])[CH:5]=[CH:4][CH:3]=1.[CH3:13]C(=O)CCCCCCCCCCC>O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C1(C)C=CC=CC=1>[NH:1]1[C:2]2=[C:11]3[C:6](=[CH:5][CH:4]=[CH:3]2)[CH:7]=[CH:8][CH:9]=[C:10]3[NH:12][CH2:13]1

참가 물질

5

반응물 2

HCID 116222-TridecanoneHCID 680671,8-Diaminonaphthalene

생성물 1

HCID 124409652,3-Dihydroperimidine수율 174.3%

시약·촉매·용매 2

HCID 521998p-Toluenesulfonic acid monohydrate촉매HCID 1140Toluene용매

실험 절차

A stirred mixture of 26.05 g of 1,8-diaminonaphthalene, 32.66 g of 2-tridecanone, 55 mg of p-toluenesulfonic acid monohydrate, and 250 mL of toluene was heated to reflux under a nitrogen atmosphere using a Dean-Stark trap to remove the water evolved from the reaction for 5 hr. The mixture was then washed with saturated sodium bicarbonate solution, dried over anhydrous potassium carbonate, filtered, and the solvent removed under reduced pressure. The product was distilled to yield 48.86 g of dihydroperimidine intermediate, bp 192°-213° C. at 0.3 to 0.4 torr.

후처리

  1. temperaturewas heated
  2. temperatureto reflux under a nitrogen atmosphere
  3. customto remove the water
  4. customevolved from the reaction for 5 hr
  5. washThe mixture was then washed with saturated sodium bicarbonate solution
  6. dry with materialdried over anhydrous potassium carbonate
  7. filtrationfiltered
  8. customthe solvent removed under reduced pressure
  9. distillationThe product was distilled

출처 및 근거

ORD 기록
ord-e3e45563951a4d36ac60f60d1d047019
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05380635

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