Acetic Anhydride → HCID 59299958, 화합물

HRID 2236564노트

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HRID 2236564 반응식
[CH3:1][N:2]1[C:11](=[O:12])[CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]1=[O:13].C[C:15]([O:17][C:18](C)=O)=O.C(OC)(OC)OC>CN(C)C=O>[CH3:1][N:2]1[C:11](=[O:12])/[C:10](=[CH:15]/[O:17][CH3:18])/[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]1=[O:13]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 9005Trimethyl orthoformateHCID 3494362-Methylisoquinoline-1,3(2H,4H)-dione

생성물 1

HCID 59299958HCID 59299958, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
125 °C

실험 절차

To a stirred mixture of 0.35 g (2.0 mmol) of (N-methyl)isoquinoline-1,3(2H,4H)-dione, 3.2 ml of Ac2O, and 0.80 ml of N,N-DIMETHYLFORMAMIDE (DMF) is added 0.44 ml (4.0 mmol) of (MeO)3CH at 25° C. The mixture is stirred at 125° C. for 30 m, cooled, and concentrated under high vacuum. The residue is recrystallized from Et2O-hexane to give 0.20 g of tan solid, mp 145-150° C. (dec); MS (ES+) m/z 218.2 (M+H)+1.

후처리

  1. temperaturecooled
  2. concentrationconcentrated under high vacuum
  3. customThe residue is recrystallized from Et2O-hexane

출처 및 근거

ORD 기록
ord-5651e3332ec240e5958fdc13196708a7
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713994B2

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