1-Isopropylhydrazine hydrochloride → 10-bromo-2-(1-isopropyl-1H-1,2,4-triazol-5-yl)-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine

HRID 1530541노트

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HRID 1530541 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](/[N:18]=[CH:19]/[N:20](C)C)=O)=[CH:10]3)=[CH:4][CH:3]=1.Cl.[CH:24]([NH:27]N)([CH3:26])[CH3:25]>CC(O)=O>[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]2[N:27]([CH:24]([CH3:26])[CH3:25])[N:20]=[CH:19][N:18]=2)=[CH:10]3)=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 855731-Isopropylhydrazine hydrochlorideHCID 178484339HCID 178484339, 화합물

생성물 1

HCID 5820501010-bromo-2-(1-isopropyl-1H-1,2,4-triazol-5-yl)-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine수율 78.8%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
100 °C

실험 절차

To a solution of 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, 6.1 mmol) in AcOH (20 mL) was added isopropylhydrazine hydrochloride (0.73 g, 6.6 mmol). The mixture was heated at 100° C. for 1 h. Most of the solvent was removed and water (50 mL) was added. The solid was collected by filtration, washed with water, and dried in vacuo to afford the title compound (1.8 g, 74% yield) as a yellow solid. LCMS m/z [M+H]+ 376.1.

후처리

  1. customMost of the solvent was removed
  2. additionwater (50 mL) was added
  3. filtrationThe solid was collected by filtration
  4. washwashed with water
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-bd4512caa7fe4b63b07d24c3dfa28ce5
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09090628B2

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