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Hydrochloric Acid → HCID 58190473, 화합물

HRID 1892384
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HRID 1892384 반응식
O.NN.[O:4]([N:11]1C(=O)C2[C:13](=CC=CC=2)[C:12]1=O)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[N:22]1[C:31]2[C:26](=[CH:27][C:28]([CH2:32][C:33]3[N:37]4[N:38]=[C:39](C(=O)C)[CH:40]=[CH:41][C:36]4=[N:35][N:34]=3)=[CH:29][CH:30]=2)[CH:25]=[CH:24][CH:23]=1.Cl>CO>[C:5]1([O:4]/[N:11]=[C:12](/[C:39]2[CH:40]=[CH:41][C:36]3[N:37]([C:33]([CH2:32][C:28]4[CH:27]=[C:26]5[C:31](=[CH:30][CH:29]=4)[N:22]=[CH:23][CH:24]=[CH:25]5)=[N:34][N:35]=3)[N:38]=2)\[CH3:13])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 3560555N-phenoxyphthalimideHCID 581904611-(3-(Quinolin-6-ylmethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)ethanone

생성물 1

HCID 58190473HCID 58190473, 화합물수율 59%

시약·촉매·용매 1

HCID 887
Methanol
용매

실험 절차

Hydrazine monohydrate (5.45 mg, 0.109 mmol) was added to a solution of 2-phenoxyisoindoline-1,3-dione (Organic Lett, 2001, 31, 139) (30.8 mg, 0.129 mmol) in 10 mL of MeOH. The solution was heated at reflux for 2 h and then cooled to rt. White precipitate was filtered off and 1-(3-(quinolin-6-ylmethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)ethanone (41.2) (30 mg, 0.1 mmol) was added. The pH value of solution was adjusted to 5-6 with 1N HCl solution. The reaction solution was then stirred at it overnight. Solvent was evaporated and the crude was purified by HPLC (acidic with 0.05% TFA) to give 23 mg (59%) of the title compound as a white solid (TFA salt). 1H-NMR (400 MHz, CDCl3) δ ppm 9.23 (d, 1H), 8.68 (d, 1H), 8.53 (d, 1H), 8.15 (m, 3H), 8.04 d, 1H), 7.83 (m, 1H), 7.40 (t, 2H), 7.29 (m, 2H), 7.15 (t, 1H), 4.92 (s, 2H), 2.56 (s, 3H). LC-MS (method H): [MH]+=395.2, tR=2.42 min.

후처리

  1. temperatureThe solution was heated
  2. temperatureat reflux for 2 h
  3. filtrationWhite precipitate was filtered off
  4. customSolvent was evaporated
  5. customthe crude was purified by HPLC (acidic with 0.05% TFA)

출처 및 근거

ORD 기록
ord-bdadecdff2de4e88b150d97779dcc48a
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08507676B2

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