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3-Amino-5-methylisoxazole → 1-Oxo-N-(3-phenyl-1,2-oxazol-5-yl)-2,3,4,5-tetrahydro-1H-[1,4]diazepino[1,2-a]benzimidazole-8-carboxamide

HRID 1521757
ノート
印刷プレビュー

反応式

HRID 1521757 の反応式
[O:1]=[C:2]1[C:8]2=[N:9][C:10]3[CH:15]=[CH:14][C:13]([C:16]([OH:18])=O)=[CH:12][C:11]=3[N:7]2[CH2:6][CH2:5][CH2:4][NH:3]1.C(N1C=CN=C1)([N:21]1C=CN=C1)=O.C[C:32]1[O:36][N:35]=[C:34](N)[CH:33]=1.[CH2:38]1[CH2:48][CH2:47]N2[C:41](=NCCC2)[CH2:40][CH2:39]1>C1COCC1>[O:1]=[C:2]1[C:8]2=[N:9][C:10]3[CH:15]=[CH:14][C:13]([C:16]([NH:21][C:32]4[O:36][N:35]=[C:34]([C:38]5[CH:39]=[CH:40][CH:41]=[CH:47][CH:48]=5)[CH:33]=4)=[O:18])=[CH:12][C:11]=3[N:7]2[CH2:6][CH2:5][CH2:4][NH:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 661723-Amino-5-methylisoxazoleHCID 682631,1'-CarbonyldiimidazoleHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 672364761-Oxo-2,3,4,5-tetrahydro-1H-[1,4]diazepino[1,2-a]benzimidazole-8-carboxylic acid2 回

生成物 1

HCID 683226701-Oxo-N-(3-phenyl-1,2-oxazol-5-yl)-2,3,4,5-tetrahydro-1H-[1,4]diazepino[1,2-a]benzimidazole-8-carboxamide収率 15.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 1-oxo-2,3,4,5-tetrahydro-1H-[1,4]diazepino[1,2-a]benzimidazole-8-carboxylic acid (Intermediate B, 71 mg, 0.29 mmol) and 1,1′-carbonyldiimidazole (117 mg, 0.72 mmol) in THF (10 mL) is heated to 60° C. for 1 h. The solution is cooled to room temperature and 5-methyl-3-aminoisoxazole (191 mg, 1.16 mmol) is added. After 10 min DBU (0.11 mL, 0.72 mmol) is added and the mixture heated at 60° C. for 16 h. The solvent is evaporated and H2O is added to the residue. The resulting solid is collected by filtration and is purified via preparative HPLC to afford the title compound (17 mg, 12%).

後処理

  1. temperaturethe mixture heated at 60° C. for 16 h
  2. customThe solvent is evaporated
  3. additionH2O is added to the residue
  4. filtrationThe resulting solid is collected by filtration
  5. customis purified via preparative HPLC

出典と根拠

ORDレコード
ord-d00844fc9eae48cdb4ae60ac5c475ce5
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09073926B2

反応ノート

読み込み中…

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