Dimethylformamide dimethyl acetal → HCID 178484339, 화합물

HRID 1530533노트

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HRID 1530533 반응식
[Br:1][C:2]1[CH:15]=[C:14]2[C:5]([O:6][CH2:7][CH2:8][N:9]3[C:13]2=[N:12][C:11]([C:16]([NH2:18])=[O:17])=[CH:10]3)=[CH:4][CH:3]=1.[CH3:19][N:20]([CH:22](OC)OC)[CH3:21]>O1CCOCC1>[Br:1][C:2]1[CH:15]=[C:14]2[C:5]([O:6][CH2:7][CH2:8][N:9]3[C:13]2=[N:12][C:11]([C:16](/[N:18]=[CH:19]/[N:20]([CH3:22])[CH3:21])=[O:17])=[CH:10]3)=[CH:4][CH:3]=1

참가 물질

4

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HCID 78373Dimethylformamide dimethyl acetalHCID 6831288310-Bromo-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine-2-carboxamide

생성물 1

HCID 178484339HCID 178484339, 화합물수율 93.2%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

To a solution of 13-bromo-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaene-4-carboxamide (2.0 g, 6.5 mmol) in dioxane (30 mL) was added DMF-DMA (2.6 mL, 19 mmol). The reaction mixture was heated at 100° C. for 1 h. The solvent was removed under reduce pressure and the residue was triturated with hot diethyl ether. The solid was collected by filtration, washed with diethyl ether and dried in vacuo to afford 13-Bromo-N-[(1E)-(dimethylamino)methylidene]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaene-4-carboxamide (2.2 g, 93% yield) as a yellow solid. LCMS (ESI) m/z: 365.1 [M+H+]

후처리

  1. customThe solvent was removed
  2. customthe residue was triturated with hot diethyl ether
  3. filtrationThe solid was collected by filtration
  4. washwashed with diethyl ether
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-71dd046e9a6b4e2fac1c8a1d1ad6f853
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09090628B2

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