1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) → HCID 67417406, 화합물

HRID 1803620

반응식

HRID 1803620 반응식
[C:1]([N:8]1[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].BrC1[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][C:17]=1[C:18]#[N:19].CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2.CC(C)([O-])C.[Na+]>O1CCOCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[C:4]([O:3][C:1]([N:8]1[CH2:9][CH2:10][N:11]([C:12]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][C:17]=2[C:18]#[N:19])[CH2:13][CH2:14]1)=[O:2])([CH3:5])([CH3:6])[CH3:7]

참가 물질

7

반응물 4

HCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 2756058Tert-butyl 1,4-diazepane-1-carboxylateHCID 217840962-Bromo-5-methoxybenzonitrileHCID 23676156Sodium t-butoxide

생성물 1

HCID 67417406HCID 67417406, 화합물수율 92.3%

시약·촉매·용매 2

HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 312751,4-Dioxane용매

반응 조건

온도
90 °C

실험 절차

A mixture of Boc-homopiperazine (483 mg, 2.59 mmol), 2-bromo-5-methoxybenzonitrile (500 mg, 2.36 mmol), Pd2(dba)3 (108 mg, 0.12 mmol), xantphos (205 mg, 0.35 mmol), sodium t-butoxide (666 mg, 7.08 mmol) in degassed anhydrous dioxane (10 mL) was heated at 90° C. for 2 h. The mixture was allowed to cool and filtered through celite. The filtrate was concentrated and purified by chromatography (EtOAc/hexanes) to yield the title compound (691 mg, 92%). m/z (M+1) 318.39.

후처리

  1. temperatureto cool
  2. filtrationfiltered through celite
  3. concentrationThe filtrate was concentrated
  4. custompurified by chromatography (EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-7e9c72ccfe004b5ea75fd268cf53da6f
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08349836B2

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