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1-Tert-butyl 3-methyl 4-(trifluoromethanesulfonyloxy)-1,2,5,6-tetrahydropyridine-1,3-dicarboxylate → HCID 58248373、化合物

HRID 2065767
ノート
印刷プレビュー

反応式

HRID 2065767 の反応式
[Cl-].[CH3:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[Zn+].C1(C)C=CC=CC=1[Mg]Cl.[CH3:19][O:20][C:21]([C:23]1[CH2:24][N:25]([C:37]([O:39][C:40]([CH3:43])([CH3:42])[CH3:41])=[O:38])[CH2:26][CH2:27][C:28]=1OS(C(F)(F)F)(=O)=O)=[O:22]>C1COCC1.[Cl-].[Zn+2].[Cl-].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:19][O:20][C:21]([C:23]1[CH2:24][N:25]([C:37]([O:39][C:40]([CH3:43])([CH3:42])[CH3:41])=[O:38])[CH2:26][CH2:27][C:28]=1[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[CH3:2])=[O:22]
参加物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 152219361-Tert-butyl 3-methyl 4-(trifluoromethanesulfonyloxy)-1,2,5,6-tetrahydropyridine-1,3-dicarboxylateHCID 178424304HCID 178424304、化合物HCID 178424428HCID 178424428、化合物

生成物 1

HCID 58248373HCID 58248373、化合物

試薬・触媒・溶媒 3

HCID 3007855Zincchloride触媒
HCID 178418397
HCID 178418397、化合物
触媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 2-methylphenylzinc chloride ([84109-17-1], previously prepared from o-tolylmagnesium chloride (44.07 mL) and zinc chloride (8.81 g) in THF (200 mL)) a mixture of 4-trifluoromethanesulfonyloxy-5,6-dihydro-2H-pyridine-1,3-dicarboxylic acid 1-tert-butyl ester 3-methyl ester (CAS Reg. No. [161491-25-4]) (11.4 g) in THF (90 mL) followed by tetrakis(triphenylphosphine)palladium(0) (1.02 g) was added. The reaction mixture was stirred at room temperature over night and then was quenched with ice. The mixture was diluted with tert-butyl methyl ether and washed with 2 M aqueous sodium carbonate solution. The aqueous phases were extracted with tert-butyl methyl ether. The combined organic layers were washed with brine, dried (Na2SO4), filtered and evaporated. Purification by chromatography (SiO2, n-heptane/ethyl acetate 5:1) gave 4-o-tolyl-5,6-dihydro-2H-pyridine-1,3-dicarboxylic acid 1-tert-butyl ester 3-methyl ester as light yellow oil, MS: 332.0 ([M+H])+.

後処理

  1. additionwas added
  2. customwas quenched with ice
  3. additionThe mixture was diluted with tert-butyl methyl ether
  4. washwashed with 2 M aqueous sodium carbonate solution
  5. extractionThe aqueous phases were extracted with tert-butyl methyl ether
  6. washThe combined organic layers were washed with brine
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. customevaporated
  10. customPurification by chromatography (SiO2, n-heptane/ethyl acetate 5:1)

出典と根拠

ORDレコード
ord-6400119517dd4c2da4c2252f12abf657
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08288541B2

反応ノート

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