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tert-Butyl piperazine-1-carboxylate → 1-(4-Chloro-3-isopropoxy-phenyl)-piperazine

HRID 1371983
ノート
印刷プレビュー

反応式

HRID 1371983 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[C:4]([O:9][CH:10]([CH3:12])[CH3:11])[CH:3]=1.C([N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1)(OC(C)(C)C)=O.CC(C)([O-])C.[Na+]>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]>[Cl:8][C:5]1[CH:6]=[CH:7][C:2]([N:20]2[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)=[CH:3][C:4]=1[O:9][CH:10]([CH3:12])[CH3:11]
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

5

反応物 3

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 210710294-Bromo-1-chloro-2-isopropoxybenzeneHCID 23676156Sodium t-butoxide

生成物 1

HCID 210710221-(4-Chloro-3-isopropoxy-phenyl)-piperazine

試薬・触媒・溶媒 1

HCID 9811564Bis(dibenzylideneacetone)palladium触媒

反応条件

温度
85 °C

実験手順

1-Bromo-3-isopropoxy-4-chlorobenzene (preparation described elsewhere) was combined with 1.11 g (6 mmol) of 1-Bocpiperazine, 672 mg (7.0 mmol) of sodium tert-butoxide, 93 mg (0.15 mmol) of rac-2,2′-Bis(diphenylphosphine)-1,1′-binaphthyl, and 45 mg (0.05 mmol) Tris(dibenzylideneacetone)dipalladium (0) in a flask under an N2 atmosphere, and the mixture was heated at 85° C. for 3.5 hours. The resulting residue was partitioned between a 1/1 mixture of ether and ethyl acetate and water, and the phases were separated. The ether/ethyl acetate phase was diluted with one volume of hexanes, washed twice with 0.5M pH=7 phosphate buffer, and once each with 1M NaOH and brine. The final organic phase was dried over Na2SO4, filtered, and concentrated in vacuo to an oil. The oil was dissolved in ethyl acetate, 10 mL each of 2M HCl in ether and methanol were added, and the product was isolated by filtration after crystallization. 1H NMR (D2O, 400 MHz): 7.23 (d, 1H), 6.69 (s, 1H), 6.59 (d, 1H), 4.53 (m, 1H), 3.28 (m, 8H), 1.20 (d, 6H) ppm.

後処理

  1. customThe resulting residue was partitioned between a 1/1 mixture of ether and ethyl acetate and water
  2. customthe phases were separated
  3. additionThe ether/ethyl acetate phase was diluted with one volume of hexanes
  4. washwashed twice with 0.5M pH=7 phosphate buffer
  5. dry with materialThe final organic phase was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo to an oil
  8. dissolutionThe oil was dissolved in ethyl acetate
  9. addition10 mL each of 2M HCl in ether and methanol were added
  10. customthe product was isolated by filtration
  11. customafter crystallization

出典と根拠

ORDレコード
ord-7f59b23909004ef98bbd2fd00098abf2
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07157464B2

反応ノート

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