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Benzylamine → cis-6-Benzylamino-8-methyl-1,2,4,4a,9,9a-hexahydro-3-aza-fluorene-3-carboxylic acid ethyl ester

HRID 1714153
ノート
印刷プレビュー

反応式

HRID 1714153 の反応式
[CH2:1]([O:3][C:4]([N:6]1[CH2:18][C@H:17]2[C@H:9]([CH2:10][C:11]3[C:16]2=[CH:15][C:14](Br)=[CH:13][C:12]=3[CH3:20])[CH2:8][CH2:7]1)=[O:5])[CH3:2].[CH2:21]([NH2:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.CC([O-])(C)C.[Na+]>C1(C)C=CC=CC=1.C(Cl)Cl.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]>[CH2:1]([O:3][C:4]([N:6]1[CH2:18][C@H:17]2[C@H:9]([CH2:10][C:11]3[C:16]2=[CH:15][C:14]([NH:28][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[CH:13][C:12]=3[CH3:20])[CH2:8][CH2:7]1)=[O:5])[CH3:2]
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

7

反応物 3

HCID 7504BenzylamineHCID 23676156Sodium t-butoxideHCID 86611065cis-6-Bromo-8-methyl-1,2,4,4a,9,9a-hexahydro-3-aza-fluorene-3-carboxylic acid ethyl ester

生成物 1

HCID 86611066cis-6-Benzylamino-8-methyl-1,2,4,4a,9,9a-hexahydro-3-aza-fluorene-3-carboxylic acid ethyl ester収率 90%

試薬・触媒・溶媒 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 1140Toluene溶媒
HCID 6344Dichloromethane溶媒

反応条件

温度
80 °C

実験手順

cis-6-Bromo-8-methyl-1,2,4,4a,9,9a-hexahydro-3-aza-fluorene-3-carboxylic acid ethyl ester (68 mg, 0.2 mmol), benzylamine (64 mg, 0.6 mmol), NaOt-Bu (58 mg, 0.3 mmol) and (2-biphenyl)di-t-butylphosphine (11 mg, 0.018 mmol) were dissolved in toluene (5.0 mL), and the solution was degassed. To the solution was added tris(dibenzylideneacetone)dipalladium (11 mg, 0.006 mmol), and the reaction mixture was heated at 80° C. for 15 h under Ar. The reaction mixture was cooled to 20° C. and diluted with CH2Cl2. The organic layer was washed with brine, dried over MgSO4, filtered and concentrated in vacuo. The residue was filtered through short silica gel column (Hex/EtOAc 7/3) to obtain crude cis-6-benzylamino-8-methyl-1,2,4,4a,9,9a-hexahydro-3-aza-fluorene-3-carboxylic acid ethyl ester (66 mg, 0.18 mmol)

後処理

  1. customthe solution was degassed
  2. temperatureThe reaction mixture was cooled to 20° C.
  3. washThe organic layer was washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. filtrationThe residue was filtered through short silica gel column (Hex/EtOAc 7/3)

出典と根拠

ORDレコード
ord-8086119f58564dfa9dcb73d2a4021db7
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07795436B2

反応ノート

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