Hydrazine hydrate (1:1) → HCID 178452593、化合物

HRID 1509153ノート

反応式

HRID 1509153 の反応式
[C:1]([O:5][C:6](=[O:35])[NH:7][C:8]1([C:12]2[CH:17]=[CH:16][C:15]([C:18]3[C:19]([C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)=[CH:20][C:21]4[NH:26][C:25](=S)[CH2:24][O:23][C:22]=4[N:28]=3)=[CH:14][CH:13]=2)[CH2:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].O.[NH2:37][NH2:38]>C1COCC1>[C:1]([O:5][C:6](=[O:35])[NH:7][C:8]1([C:12]2[CH:17]=[CH:16][C:15]([C:18]3[C:19]([C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)=[CH:20][C:21]4[NH:26]/[C:25](=[N:37]/[NH2:38])/[CH2:24][O:23][C:22]=4[N:28]=3)=[CH:14][CH:13]=2)[CH2:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 86683631Tert-butyl (1-(4-(7-phenyl-2-thioxo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-6-yl)phenyl)cyclobutyl)carbamate

生成物 1

HCID 178452593HCID 178452593、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of tert-butyl(1-(4-(7-phenyl-2-thioxo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-6-yl)phenyl)cyclobutyl)carbamate (2 g, 2.05 mmol) in THF (350 mL) was added hydrazine monohydrate (645 μl, 20.51 mmol) to give a yellow solution. The resulting mixture was stirred at room temperature for 2 hours. The mixture was filtered to remove insoluble black particles and concentrated to dryness under reduced pressure. The resulting yellow solid was used directly in the following step as crude without any further purification. LCMS (Method D): RT=1.04 min, M+1=486.

後処理

  1. customto give a yellow solution
  2. filtrationThe mixture was filtered
  3. customto remove insoluble black particles
  4. concentrationconcentrated to dryness under reduced pressure
  5. customThe resulting yellow solid was used directly in the following step as crude without any further purification

出典と根拠

ORDレコード
ord-5ae326018fa045cf9701e07ac78652bf
出典データセット
uspto-grants-2015_12
特許番号
US09221838B2

反応ノート

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