Sodium Hydroxide → 1-(3-Methylanilino)phthalazine-4-carbaldehyde

HRID 2119300노트

반응식

HRID 2119300 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH:22]=[CH:23][CH:24]=1)[NH:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([CH:16]2OCOC[O:17]2)=[N:8][N:7]=1.[OH-].[Na+]>OS(O)(=O)=O>[CH3:1][C:2]1[CH:3]=[C:4]([CH:22]=[CH:23][CH:24]=1)[NH:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([CH:16]=[O:17])=[N:8][N:7]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 223864601-(3-Methylanilino)-4-([1,3,5]trioxan-2-yl)phthalazine

생성물 1

HCID 223864531-(3-Methylanilino)phthalazine-4-carbaldehyde

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

반응 조건

온도
100 °C

실험 절차

A suspension of 3.15 g (9.74 mmol) 1-(3-methylanilino)-4-([1,3,5]trioxan-2-yl)phthalazine in 150 ml H2SO4 (10% in H2O) is stirred for 7 h at 100° C. The suspension is cooled to RT and adjusted to alkaline pH with NaOH (20% in H2O), the title compound that precipitates out is filtered off and washed with water; 1H-NMR (DMSO-d6) 10.17 (s, HCO), 9.84 (s, HN), 9.02 (d, 1H), 8.67 (d, 1H), 8.03 (m, 2H), 7.8-7.6 (2 sb, 2H), 7.30 (t, 1H), 6.98 (d, 1H), 2.36 (s, 3H); FAB-MS (M−H)+=262.

후처리

  1. temperatureThe suspension is cooled to RT
  2. customthe title compound that precipitates out
  3. filtrationis filtered off
  4. washwashed with water

출처 및 근거

ORD 기록
ord-617a7effc809405c9ab75c7c9cadfeff
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06686347B2

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