Dimethyl Phthalate → HCID 178509848, 화합물

HRID 365472

반응식

HRID 365472 반응식
[Br-].C(OC[N+:10]1[CH:14]=[C:13]([CH2:15][CH2:16][N:17]2C(=O)C3=CC=CC=C3[C:18]2=O)[N:12](CC2C=CC(C#N)=CC=2)[CH:11]=1)(=O)C(C)(C)C.[NH2:37]N.C(OC)(=O)[C:40]1[C:41](=[CH:46][CH:47]=[CH:48][CH:49]=1)[C:42](OC)=O>C(O)C>[C:42]([C:41]1[CH:40]=[CH:49][C:48]([CH2:18][NH:17][CH2:16][CH2:15][C:13]2[N:12]=[CH:11][NH:10][CH:14]=2)=[CH:47][CH:46]=1)#[N:37]

참가 물질

5

반응물 3

HCID 8554Dimethyl PhthalateHCID 9321HydrazineHCID 86755883HCID 86755883, 화합물

생성물 1

HCID 178509848HCID 178509848, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1-Pivaloyloxymethyl-3-(4-cyanobenzyl)-4-(2-phthalimidoethyl) imidazolium bromide (1.00 g, 1.81 mmol) was dissolved in ethanol (50 mL), treated with hydrazine (0.287 mL, 9.06 mmol), and heated at reflux for 16 h. Dimethyl phthalate (2.22 mL, 13.57 mmol) was added and reflux was continued for 6 h. The reaction mixture was cooled in an ice-H2O bath, the solid precipitate filtered off, the filtrate concentrated to dryness, and the residue chromatographed (SiO2, CH2Cl2 (NH4OH): 3-8% CH3OH) to give the title compound. 1H NMR (CD3OD) δ 7.76 (s, 1H), 7.74 (d, 2H, J=8 Hz), 7.27 (d, 2H, J=8 Hz), 6.88 (s, 1H), 5.35 (s, 2H), 2.76 (t, 2H, J=6 Hz), 2.60 (t, 2 H, J=6 Hz).

후처리

  1. temperatureheated
  2. temperatureat reflux for 16 h
  3. temperaturereflux
  4. temperatureThe reaction mixture was cooled in an ice-H2O bath
  5. filtrationthe solid precipitate filtered off
  6. concentrationthe filtrate concentrated to dryness
  7. customthe residue chromatographed (SiO2, CH2Cl2 (NH4OH): 3-8% CH3OH)

출처 및 근거

ORD 기록
ord-3bd4b4962be24736b720693d111001fd
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06127390

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