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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Triethylamine → HCID 21477601、化合物

HRID 864394
ノート
印刷プレビュー

反応式

HRID 864394 の反応式
[CH3:1][C:2]([CH3:23])([O:4][C:5]([N:7]1[CH2:12][CH2:11][N:10]([C:13]2[N:18]=[CH:17][N:16]=[C:15](Cl)[C:14]=2[N+:20]([O-])=O)[CH2:9][CH2:8]1)=[O:6])[CH3:3].C(N(CC)CC)C.[H][H]>[Pd].C(O)C>[CH3:3][C:2]([CH3:23])([O:4][C:5]([N:7]1[CH2:8][CH2:9][N:10]([C:13]2[N:18]=[CH:17][N:16]=[CH:15][C:14]=2[NH2:20])[CH2:11][CH2:12]1)=[O:6])[CH3:1]
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 3

HCID 8471TriethylamineHCID 21477639tert-Butyl 4-(6-chloro-5-nitropyrimidin-4-yl)piperazine-1-carboxylateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 21477601HCID 21477601、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A mixture of 1-[1,1-dimethylethoxycarbonyl]-4-[4-chloro-5-nitro-6-pyrimidyl]piperazine (PREPARATION 23, 0.56 g) and triethylamine (0.3 ml) and palladium on carbon (5%, 0.13 g) in ethanol (100 ml) is charged with hydrogen gas (30 psi). After the theoretical amount of hydrogen gas is consumed, the catalyst is removed under reduced pressure. The filtrate is concentrated under reduced pressure to a foam which is diluted with an aqueous saturated solution of potassium carbonate and dichloromethane. The phases are separated and the organic phase is dried over sodium sulfate and concentrated to give to give the title compound, NMR (CDCl3) 1.49, 3.49, 3.29, 3.56, 7.98, and 8.39δ.

後処理

  1. customAfter the theoretical amount of hydrogen gas is consumed
  2. customthe catalyst is removed under reduced pressure
  3. concentrationThe filtrate is concentrated under reduced pressure to a foam which
  4. additionis diluted with an aqueous saturated solution of potassium carbonate and dichloromethane
  5. customThe phases are separated
  6. dry with materialthe organic phase is dried over sodium sulfate
  7. concentrationconcentrated
  8. customto give

出典と根拠

ORDレコード
ord-17b9fce27bbb4594a1780df6322afe6d
出典データセット
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05563142

反応ノート

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