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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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Methanol → 2-[(4-Fluorophenyl)methyl]-7,8-dihydro-10-hydroxy-8-methylpyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione

HRID 494105
ノート
印刷プレビュー

反応式

HRID 494105 の反応式
Br[C:2]1[C:3](=[O:24])[N:4]([CH2:16][C:17]2[CH:22]=[CH:21][C:20]([F:23])=[CH:19][CH:18]=2)[N:5]=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][N:11]([CH3:14])[C:10](=[O:15])[CH2:9]1.C1(C(N)C2CCCCC2)CCCCC1.[CH3:39][OH:40]>CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C>[F:23][C:20]1[CH:21]=[CH:22][C:17]([CH2:16][N:4]2[C:3](=[O:24])[C:2]3[C:39]([OH:40])=[C:9]4[C:10](=[O:15])[N:11]([CH3:14])[CH2:12][CH2:13][N:8]4[C:7]=3[CH:6]=[N:5]2)=[CH:18][CH:19]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887Methanol2 回HCID 10774245alpha-CyclohexylcyclohexanemethanamineHCID 68867528HCID 68867528、化合物

生成物 1

HCID 546779322-[(4-Fluorophenyl)methyl]-7,8-dihydro-10-hydroxy-8-methylpyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione

試薬・触媒・溶媒 1

HCID 178418851HCID 178418851、化合物触媒

反応条件

温度
90 °C

実験手順

A mixture of 4-bromo-2-(4-fluorobenzyl)-5-(4-methyl-3-oxopiperazin-1-yl)pyridazin-3(2H)-one (0.2 g, 0.51 mmol), dicyclohexylmethylamine (0.15 g, 0.76 mmol), and bis-(tri-t-butylphosphine)palladium (0) (52 mg, 0.10 mmol) in anhydrous methanol (5 mL) was heated in a stainless steel pressure vessel under an atmosphere of carbon monoxide (250 psi) in an oil bath at 90° C. overnight. The resultant mixture was diluted with methanol, filtered through a pad of Celite. The filtrate was concentrated under vacuum. The residual oil was triturated with methanol. The white solid precipitated was filtered to provide the titled dione.

後処理

  1. filtrationfiltered through a pad of Celite
  2. concentrationThe filtrate was concentrated under vacuum
  3. customThe residual oil was triturated with methanol
  4. customThe white solid precipitated
  5. filtrationwas filtered
  6. customto provide the titled dione

出典と根拠

ORDレコード
ord-1787552fdde342afbbc82afabdb147ec
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07538112B2

反応ノート

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