Dimethylformamide dimethyl acetal → HCID 178484342, 화합물

HRID 1530518노트

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HRID 1530518 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:13](=[CH:14][N:15]=1)[C:12]1[N:8]([CH:9]=[C:10]([C:16]([NH2:18])=[O:17])[N:11]=1)[CH2:7][CH2:6][O:5]2.[CH3:19][N:20]([CH:22](OC)OC)[CH3:21]>O1CCOCC1>[Cl:1][C:2]1[CH:3]=[C:4]2[C:13](=[CH:14][N:15]=1)[C:12]1[N:8]([CH:9]=[C:10]([C:16](/[N:18]=[CH:19]/[N:20]([CH3:22])[CH3:21])=[O:17])[N:11]=1)[CH2:7][CH2:6][O:5]2

참가 물질

4

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HCID 78373Dimethylformamide dimethyl acetalHCID 582042888-Chloro-4,5-dihydro-6-oxa-1,3a,9-triaza-benzo[e]azulene-2-carboxylic acid amide

생성물 1

HCID 178484342HCID 178484342, 화합물수율 68%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

To a solution of 12-chloro-9-oxa-3,6,13-triazatricyclo[8.4.0.02,6]tetradeca-1(14),2,4,10,12-pentaene-4-carboxamide (0.380 mmol, 100 mg) in 1,4-dioxane (3 mL) was added DMF-DMA (1.14 mmol, 147 mg). The mixture was stirred at 100° C. for 1 hour under nitrogen atmosphere. Then solvent was evaporated under reduced pressure, the residue was washed by ether to give 12-chloro-N-[(1E)-(dimethylamino)methylidene]-9-oxa-3,6,13-triazatricyclo[8.4.0.02,6]tetradeca-1(14),2,4,10,12-pentaene-4-carboxamide (80 mg, 68% yield), which was used in the next step without further purification. LCMS (ESI) m/z: 320.1 [M+H+]

후처리

  1. customThen solvent was evaporated under reduced pressure
  2. washthe residue was washed by ether

출처 및 근거

ORD 기록
ord-4b160a2242c44106b7d7d549b94ab245
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09090628B2

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