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Hydrochloric Acid → HCID 86622859、化合物

HRID 1013124
ノート
印刷プレビュー

反応式

HRID 1013124 の反応式
ClC1C=CC2CCN(C(=O)C(F)(F)F)CCC=2C=1OS(C(F)(F)F)(=O)=O.CC1(CCCN)OCCO1.C1(P(C2C=CC=CC=2)C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(=O)([O-])[O-].[Cs+].[Cs+].[Cl:89][C:90]1[CH:106]=[CH:105][C:93]2[CH2:94][CH2:95][N:96]([C:99](=[O:104])[C:100]([F:103])([F:102])[F:101])[CH2:97][CH2:98][C:92]=2[C:91]=1[NH:107][CH2:108][CH2:109][CH2:110][C:111]1([CH3:116])OCCO1.Cl.C([BH3-])#N.[Na+]>C1(C)C=CC=CC=1.CCOC(C)=O.C(Cl)Cl.C(OCC)C.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].CO>[Cl:89][C:90]1[CH:106]=[CH:105][C:93]2[CH2:94][CH2:95][N:96]([C:99](=[O:104])[C:100]([F:101])([F:103])[F:102])[CH2:97][CH2:98][C:92]=2[C:91]=1[N:107]1[CH2:108][CH2:109][CH2:110][CH:111]1[CH3:116]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

14

反応物 7

HCID 313Hydrochloric AcidHCID 10796Cesium carbonateHCID 5600073-(2-Methyl-1,3-dioxolan-2-yl)-1-propanamineHCID 634876Binap, (A+-)-HCID 5003444Sodium cyanoborohydrideHCID 574477477-Chloro-3-(2,2,2-trifluoroacetyl)-6-trifluoromethylsulfonyloxy-2,3,4,5-tetrahydro-1H-benzo[d]azepine
HCID 86622860
7-chloro-3-(2,2,2-trifluoroacetyl)-6-[3-(2-methyl[1,3]dioxolan-2-yl)-propylamino]-2,3,4,5-tetrahydro-1H-benzo[d]azepine

生成物 1

HCID 86622859HCID 86622859、化合物収率 81.3%

試薬・触媒・溶媒 6

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 887Methanol溶媒HCID 1140Toluene溶媒HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
95 °C

実験手順

Place 7-chloro-3-(2,2,2-trifluoroacetyl)-6-trifluoromethanesulfonyloxy-2,3,4,5-tetrahydro-1H-benzo[d]azepine (prepared essentially as described in Preparation 1) (3 g, 7.08 mmol) in toluene (60 mL) with 3-(2-methyl-[1,3]dioxolan-2-yl)-propylamine (prepared essentially as described in Preparation 38) (3.08 g, 21.24 mmol), tris(dibenzylideneacetone)dipalladium (1.3 g, 1.42 mmol), racemic 2,2′-bis(diphenylphosphino)-1,1′-binapthyl (1.77 g, 2.84 mmol), and cesium carbonate (3.3 g, 9.91 mmol) and heat for 16 h at 95° C. in a sealed tube. Cool the reaction to RT, dilute with EtOAc (600 mL) and filter. Concentrate the filtrate and purify (silica gel chromatography, eluting with 10:90 to 25:75 EtOAc:hexanes) to give the crude product as an orange oil (1.72 g). Dissolve 7-chloro-3-(2,2,2-trifluoroacetyl)-6-[3-(2-methyl[1,3]dioxolan-2-yl)-propylamino]-2,3,4,5-tetrahydro-1H-benzo[d]azepine (1.72 g, 4.09 mmol) in DCM (20 mL) and add methanol (2 mL) and 2 N HCl in diethyl ether (20 mL) and stir at RT for 3 h. Concentrate and dissolve the residue in acetic acid (30 mL) and add sodium cyanoborohydride (1.28 g, 20.43 mmol). Stir the reaction at RT for 0.5 h then concentrate to remove the acetic acid. Dissolve the residue in DCM (200 mL) and extract with saturated aqueous sodium bicarbonate solution (400 mL), Extract the aqueous layer with DCM (100 mL) and combine the organic fractions, dry (sodium sulfate), concentrate and purify (silica gel chromatography, eluting with 10:90 EtOAc:hexanes) to give the title compound as a foam (1.2 g, 81%).

後処理

  1. customprepared essentially
  2. temperatureCool
  3. customthe reaction to RT
  4. filtrationfilter
  5. concentrationConcentrate the filtrate
  6. custompurify
  7. wash(silica gel chromatography, eluting with 10:90 to 25:75 EtOAc:hexanes)
  8. customto give the crude product as an orange oil (1.72 g)
  9. concentrationConcentrate
  10. dissolutiondissolve the residue in acetic acid (30 mL)
  11. stirringStir
  12. customthe reaction at RT for 0.5 h
  13. concentrationthen concentrate
  14. customto remove the acetic acid
  15. dissolutionDissolve the residue in DCM (200 mL)
  16. extractionextract with saturated aqueous sodium bicarbonate solution (400 mL)
  17. extractionExtract the aqueous layer with DCM (100 mL)
  18. dry with materialdry (sodium sulfate)
  19. concentrationconcentrate
  20. custompurify
  21. wash(silica gel chromatography, eluting with 10:90 EtOAc:hexanes)

出典と根拠

ORDレコード
ord-c22474ca54ec40f59dfcd8a782ea4786
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07981882B2

反応ノート

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