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Ammonium Chloride → methyl (1S,4S)-1-(2,2-difluoroethyl)-4-(2,5-dimethyl-1H-pyrrol-1-yl)cyclopent-2-ene-1-carboxylate

HRID 2067843
ノート
印刷プレビュー

反応式

HRID 2067843 の反応式
[Li+].CC([N-]C(C)C)C.[CH3:9][C:10]1[N:11]([C@H:16]2[CH2:20][C@@H:19]([C:21]([O:23][CH3:24])=[O:22])[CH:18]=[CH:17]2)[C:12]([CH3:15])=[CH:13][CH:14]=1.FC(F)(F)S(O[CH2:31][CH:32]([F:34])[F:33])(=O)=O.[NH4+].[Cl-]>C1COCC1>[F:33][CH:32]([F:34])[CH2:31][C@@:19]1([C:21]([O:23][CH3:24])=[O:22])[CH2:20][C@H:16]([N:11]2[C:10]([CH3:9])=[CH:14][CH:13]=[C:12]2[CH3:15])[CH:17]=[CH:18]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 25517Ammonium ChlorideHCID 2724682Lithium diisopropylamideHCID 27740892,2-Difluoroethyl trifluoromethanesulfonateHCID 59700297(1R,4S)-methyl 4-(2,5-dimethyl-1H-pyrrol-1-yl)cyclopent-2-enecarboxylate

生成物 1

HCID 58305966methyl (1S,4S)-1-(2,2-difluoroethyl)-4-(2,5-dimethyl-1H-pyrrol-1-yl)cyclopent-2-ene-1-carboxylate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

A −40° C. solution of 2M (in Ethylbenzene/THF/Heptane) LDA (36 ml, 72 mmol) in THF (80 ml) was placed in flask with THF (80 ml) was treated with a solution of methyl (1R,4S)-4-(2,5-dimethyl-1H-pyrrol-1-yl)cyclopent-2-ene-1-carboxylate (7.9 g, 36.3 mmol) in THF (17 ml) while keeping the temperature less than −32° C. The reaction was stirred for 30 min and then 2,2-difluoroethyl trifluoromethanesulfonate was added slowly, keeping the temperature <−28° C. The reaction was stirred with cold bath in place and allow to slowly warm. After 4 hours the reaction was poured into NH4Cl solution and extracted twice with ethyl acetate. The combined organics were washed with brine, dried over MgSO4 and concentrated to give a brown oil. The oil was passed through a column of silica gel with 10% ethyl acetate/hexanes to give methyl (1S,4S)-1-(2,2-difluoroethyl)-4-(2,5-dimethyl-1H-pyrrol-1-yl)cyclopent-2-ene-1-carboxylate as a brown oil. (7.5 g, 73%). 1H NMR (400 MHz, CDCl3) δ ppm 6.07-6.04 (1H), 6.02-6.00 (0.25H) 5.98-5.96 (1H), 5.88-5.86 (0.5H), 5.75-5.72 (2.25H), 5.36-5.30 (1H), 3.74 (3H), 2.53-2.41 (2H), 2.39-2.22 (2H), 2.19 (6H)

後処理

  1. customthe temperature less than −32° C
  2. customthe temperature <−28° C
  3. stirringThe reaction was stirred with cold bath in place
  4. temperatureto slowly warm
  5. extractionextracted twice with ethyl acetate
  6. washThe combined organics were washed with brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated
  9. customto give a brown oil

出典と根拠

ORDレコード
ord-578d9af509534ef8a7d5d5087685b383
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08293903B2

反応ノート

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