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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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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
노트
인쇄 미리보기

반응식

HRID 494105 반응식
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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887Methanol2회HCID 10774245alpha-CyclohexylcyclohexanemethanamineHCID 68867528HCID 68867528, 화합물

생성물 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

시약·촉매·용매 1

HCID 178418851HCID 178418851, 화합물촉매

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온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1787552fdde342afbbc82afabdb147ec
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07538112B2

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