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Trifluoroacetic acid → 1-[4-(3-Pyrrolidin-1-ylmethyl-cyclobutyl)-benzyl]-pyrrolidine

HRID 1241518
ノート
印刷プレビュー

反応式

HRID 1241518 の反応式
[N:1]1([CH2:6][CH:7]2[CH2:10][C:9]([C:12]3[CH:17]=[CH:16][C:15]([CH2:18][N:19]4[CH2:23][CH2:22][CH2:21][CH2:20]4)=[CH:14][CH:13]=3)(O)[CH2:8]2)[CH2:5][CH2:4][CH2:3][CH2:2]1.C(O)(C(F)(F)F)=O.C([SiH](CC)CC)C>>[N:1]1([CH2:6][CH:7]2[CH2:8][CH:9]([C:12]3[CH:13]=[CH:14][C:15]([CH2:18][N:19]4[CH2:23][CH2:22][CH2:21][CH2:20]4)=[CH:16][CH:17]=3)[CH2:10]2)[CH2:5][CH2:4][CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 219348323-Pyrrolidin-1-ylmethyl-1-(4-pyrrolidin-1-ylmethyl-phenyl)-cyclobutanol

生成物 1

HCID 113125751-[4-(3-Pyrrolidin-1-ylmethyl-cyclobutyl)-benzyl]-pyrrolidine収率 31%

実験手順

Alternatively, to a stirring solution of 3-pyrrolidin-1-ylmethyl-1-(4-pyrrolidin-1-ylmethyl-phenyl)-cyclobutanol (Example 8, General procedure B, Step D) (1.1 g, 3.5 mmol) in TFA (5.4 mL, 70.1 mmol) was added triethyl silane (5.6 mL, 35.0 mmol). The reaction was then heated to 75 □C (oil bath) for 14 hours. The reaction was then cooled to rt and concentrated under reduced pressure. The residual was taken up in CH2Cl2 and washed with NaHCO3. The aqueous layer was back extracted with 3:1 (CH3Cl:isopropanol). The combined organic layers were dried over MgSO4, filtered though a fritted funnel and concentrated under reduced pressure. Purification of this material was accomplished by flash column chromatography using a 40 M Biotage column, eluting with a gradient of 10%–20% MeOH/CH2Cl2 with 0.3% NH4OH. The product containing fractions were collected and concentrated to give the title compound (324 mg, 18%) as the bis-TFA salt. To this material in EtOAc was added a solution of HCl (2 eq, 2M THF). The resulting solution was stirred over night, and then filtered through a fritted funnel. The solid was collected and dried under reduced pressure to yield the title compound as the bis-HCl salt and as a mixture of isomers.

後処理

  1. temperatureThe reaction was then heated to 75 □C (oil bath) for 14 hours
  2. concentrationconcentrated under reduced pressure
  3. washwashed with NaHCO3
  4. extractionThe aqueous layer was back extracted with 3:1 (CH3Cl:isopropanol)
  5. dry with materialThe combined organic layers were dried over MgSO4
  6. filtrationfiltered though a fritted funnel
  7. concentrationconcentrated under reduced pressure
  8. customPurification of this material
  9. washeluting with a gradient of 10%–20% MeOH/CH2Cl2 with 0.3% NH4OH
  10. additionThe product containing fractions
  11. customwere collected
  12. concentrationconcentrated

出典と根拠

ORDレコード
ord-d806a69db99249e29d565ef27f84049c
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07115600B2

反応ノート

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