Acetic Anhydride → 2n-Octyloxy-5,12-bis(acetoxy)-tetracene

HRID 2165509노트

반응식

HRID 2165509 반응식
[CH2:1]([O:9][C:10]1[CH:27]=[CH:26][C:25]2[C:24](=[O:28])[C:23]3[C:14](=[CH:15][C:16]4[C:21]([CH:22]=3)=[CH:20][CH:19]=[CH:18][CH:17]=4)[C:13](=[O:29])[C:12]=2[CH:11]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[C:30](OC(=O)C)(=[O:32])[CH3:31].[C:37]([O-])(=[O:39])[CH3:38].[K+]>[Zn].C(OCC)(=O)C>[CH2:1]([O:9][C:10]1[CH:27]=[CH:26][C:25]2[C:12](=[C:13]([O:29][C:37](=[O:39])[CH3:38])[C:14]3[C:23]([C:24]=2[O:28][C:30](=[O:32])[CH3:31])=[CH:22][C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]=3)[CH:11]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]

참가 물질

6

반응물 3

HCID 7918Acetic AnhydrideHCID 517044Potassium AcetateHCID 200898292-n-Octyloxytetracene-5,12-dione

생성물 1

HCID 198127622n-Octyloxy-5,12-bis(acetoxy)-tetracene

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 8857Ethyl Acetate용매

실험 절차

With stirring, 2,0 g (31.05 mmol) of zinc powder are added to a mixture of 4 g (10.35 mmol) of 2-n-octyloxytetracene-5,12-dione obtained in Example 1.1., 40 ml of ethyl acetate, 25 ml of acetic anhydride and 3.05 g (31.05 mmol) of potassium acetate. The mixture is stirred for 40 minutes at 25° C. and then filtered. The residue is washed 4 times with CH2Cl2. The filtrates are connected by evaporation and the residue is recrystallised from CH2Cl2 /pentane, then from toluene. Yield: 4.1 g (84%), m.p. 107°-111° C.

후처리

  1. stirringThe mixture is stirred for 40 minutes at 25° C.
  2. filtrationfiltered
  3. washThe residue is washed 4 times with CH2Cl2
  4. customThe filtrates are connected by evaporation
  5. customthe residue is recrystallised from CH2Cl2 /pentane

출처 및 근거

ORD 기록
ord-ed5292f540534c9d802f6e67157be761
출처 데이터셋
uspto-grants-1990_07
특허 번호
US04940516

반응 노트

불러오는 중…