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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 510535
ノート
印刷プレビュー

反応式

HRID 510535 の反応式
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>[Cl:51][C:48]1[CH:49]=[CH:50][C:45]([CH2:44][CH:29]2[C:28]3[C:33](=[CH:34][CH:35]=[C:26]([CH2:12][CH2:11][CH2:10][NH:13][S:14]([CH2:17][CH2:18][CH3:19])(=[O:16])=[O:15])[CH:27]=3)[CH2:32][CH2:31][CH:30]2[NH:36][C:37](=[O:38])[O:39][C:40]([CH3:41])([CH3:42])[CH3:43])=[CH:46][CH:47]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 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

生成物 1

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

試薬・触媒・溶媒 4

HCID 167845palladium(II) acetate触媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-0535fa1d6eed4dfd81f6d58271281cd1
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09096619B2

反応ノート

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