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 1530541ノート

反応式

HRID 1530541 の反応式
[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

参加物

4

反応物 2

HCID 855731-Isopropylhydrazine hydrochlorideHCID 178484339HCID 178484339、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bd4512caa7fe4b63b07d24c3dfa28ce5
出典データセット
uspto-grants-2015_07
特許番号
US09090628B2

反応ノート

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