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Cesium carbonate → tert-Butyl [1-(4-chlorobenzyl)-7-{3-[(propylsulfonyl)amino]propyl}-1,2,3,4-tetrahydronaphthalen-2-yl]carbamate

HRID 2177102
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HRID 2177102 반응식
B1C2CCCC1CCC2.[CH2:10]([NH:13][S:14]([CH2:17][CH2:18][CH3:19])(=[O:16])=[O:15])[CH:11]=[CH2:12].FC(F)(F)S(O[C:26]1[CH:35]=[CH:34][C:33]2[CH2:32][CH2:31][CH:30]([NH:36][C:37]([O:39][C:40]([CH3:43])([CH3:42])[CH3:41])=[O:38])[CH:29]([CH2:44][C:45]3[CH:50]=[CH:49][C:48]([Cl:51])=[CH:47][CH:46]=3)[C:28]=2[CH:27]=1)(=O)=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCCC1.C(OCC)(=O)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.O1CCOCC1>[C:40]([O:39][C:37](=[O:38])[NH:36][CH:30]1[CH2:31][CH2:32][C:33]2[C:28](=[CH:27][C:26]([CH2:12][CH2:11][CH2:10][NH:13][S:14]([CH2:17][CH2:18][CH3:19])(=[O:16])=[O:15])=[CH:35][CH:34]=2)[CH:29]1[CH2:44][C:45]1[CH:50]=[CH:49][C:48]([Cl:51])=[CH:47][CH:46]=1)([CH3:43])([CH3:41])[CH3:42]
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참가 물질

10

반응물 5

HCID 10796Cesium carbonateHCID 11776TriphenylphosphineHCID 789669-Borabicyclo(3.3.1)nonaneHCID 237363N-allylpropane-1-sulfonamideHCID 574672047-(Tert-butoxycarbonylamino)-8-(4-chlorobenzyl)-5,6,7,8-tetrahydronaphthalen-2-yl trifluoromethanesulfonate

생성물 1

HCID 59547819
tert-Butyl [1-(4-chlorobenzyl)-7-{3-[(propylsulfonyl)amino]propyl}-1,2,3,4-tetrahydronaphthalen-2-yl]carbamate

시약·촉매·용매 4

HCID 167845palladium(II) acetate촉매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

To a solution of 9-BBN (0.5 M in tetrahydrofuran, 8.85 mL, 4.42 mmol) was added dropwise a solution N-allylpropane-1-sulfonamide (1152 mg, 7.06 mmol) in tetrahydrofuran (1 mL) a 0° C. After stirring at 0° C. to 5° C. for 3.5 hours dioxane (25 mL) was added followed by 7-(tert-butoxycarbonylamino)-8-(4-chlorobenzyl)-5,6,7,8-tetrahydronaphthalen-2-yl trifluoromethanesulfonate (1000 mg, 1.923 mmol, prepared analogously to example 34.3), palladium acetate (43.2 mg, 0.192 mmol), triphenylphosphine (101 mg, 0.385 mmol) and cesium carbonate (1253 mg, 3.85 mmol). The yellow reaction mixture was heated under reflux for 3 hours. The reaction mixture was diluted with ethyl acetate (60 mL) and washed with water (2×40 mL). The organic layer was dried and concentrated in vacuo. The crude product was purified by flash chromatography (silica gel, dichloro methane, methanol).

후처리

  1. additionwas added
  2. temperatureThe yellow reaction mixture was heated
  3. temperatureunder reflux for 3 hours
  4. washwashed with water (2×40 mL)
  5. customThe organic layer was dried
  6. concentrationconcentrated in vacuo
  7. customThe crude product was purified by flash chromatography (silica gel, dichloro methane, methanol)

출처 및 근거

ORD 기록
ord-2f2b25dfe34341289ee72060272557e9
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09067871B2

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