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Toluene → HCID 18186376, 화합물

HRID 1358048
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HRID 1358048 반응식
Br[C:2]1[CH:33]=[CH:32][C:5]([CH2:6][CH:7]2[C:16]3[C:11](=[CH:12][C:13]([O:17][CH2:18][C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)=[CH:14][CH:15]=3)[CH2:10][CH2:9][N:8]2[C:25]2[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=2)=[CH:4][CH:3]=1.[NH:34]1[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]1.C1(C)C=CC=CC=1.CC([O-])(C)C.[Na+]>[Cl-].[Na+].O.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].CC1C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.C(OCC)C>[N:34]1([C:2]2[CH:33]=[CH:32][C:5]([CH2:6][CH:7]3[C:16]4[C:11](=[CH:12][C:13]([O:17][CH2:18][C:19]5[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=5)=[CH:14][CH:15]=4)[CH2:10][CH2:9][N:8]3[C:25]3[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=3)=[CH:4][CH:3]=2)[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 1140TolueneHCID 8082PiperidineHCID 181864091-(4-Bromobenzyl)-2-(4-fluorophenyl)-6-(phenylmethoxy)-1,2,3,4-tetrahydroisoquinolineHCID 23676156Sodium t-butoxide

생성물 1

HCID 18186376HCID 18186376, 화합물수율 49.3%

시약·촉매·용매 4

HCID 80271
Tri-o-tolylphosphine
촉매
HCID 6505921(1E,4E)-1,5-diphenylpenta-1,4-dien-3-one; palladium촉매
HCID 3283Diethyl Ether용매
HCID 57417360Sodium chloride; water용매

실험 절차

1-(4-Bromobenzyl)-6-phenylmethoxy-2-(4-fluorophenyl)-1,2,3,4-tetrahydroisoquinoline (0.82 g, 1.6 mmol) and piperidine (0.17 g, 1.96 mmol) are placed in a 100 ml round bottom flask containing anh. toluene (50 mL) under nitrogen. NaOtBu (0.22 g, 2.3 mmol), Pd(dba)2 (0.029 g, 2 mol %) and P(o-tolyl)3 (0.02 g, 6 mol %) are added, and the mixture heated to reflux overnight. The reaction is cooled to RT and treated with brine and ethyl ether. The organic layer is dried over MgSO4 and purified by column chromatography (SiO2, hexanes/ethyl acetate, 6:1) to yield the title compound (0.40 g, 49% yield): ES-MS (m/z) 507 [M+H]+.

후처리

  1. temperaturethe mixture heated
  2. temperatureto reflux overnight
  3. dry with materialThe organic layer is dried over MgSO4
  4. custompurified by column chromatography (SiO2, hexanes/ethyl acetate, 6:1)

출처 및 근거

ORD 기록
ord-8ea45e42fd1245c1b3abb02b7b6bcd31
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06593322B1

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