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Diisopropylethylamine → HCID 86726297、化合物

HRID 1422880
ノート
印刷プレビュー

反応式

HRID 1422880 の反応式
[NH2:1][C@H:2]([C:12](=[O:20])[NH:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][S:8][C:9](=[O:11])[CH3:10].FC(F)(F)C([O-])=O.CCN(C(C)C)C(C)C.C1CN([P+](ON2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.[O:70]=[C:71]1[C@H:75]([C:76](O)=[O:77])[C@@H:74]([C:79]2[CH:84]=[CH:83][CH:82]=[CH:81][CH:80]=2)[CH2:73][NH:72]1>C(Cl)Cl.CN(C=O)C>[O:70]=[C:71]1[CH:75]([C:76]([NH:1][C@H:2]([C:12](=[O:20])[NH:13][C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][S:8][C:9](=[O:11])[CH3:10])=[O:77])[CH:74]([C:79]2[CH:84]=[CH:83][CH:82]=[CH:81][CH:80]=2)[CH2:73][NH:72]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 81531DiisopropylethylamineHCID 762604HCID 762604、化合物HCID 2724699PyBOPHCID 86726298HCID 86726298、化合物

生成物 1

HCID 86726297HCID 86726297、化合物

試薬・触媒・溶媒 1

HCID 22350042dichloromethane N,N-dimethylformamide溶媒

実験手順

Thioacetic acid S—((S)-6-amino-6-phenylcarbamoyl-hexyl) ester-trifluoroacetate (1.03 mmol), DIPEA (3.08 mmol) and PyBOP (1.03 mmol) were added to a solution of (3R*,4S*)-2-oxo-4-phenyl-pyrrolidine-3-carboxylic acid in DCM/DMF: 5/9. The resulting reaction mixture was stirred at RT overnight. After removal of the solvent under reduced pressure, the resulting solid was poured into water and extracted twice with AcOEt. The organic layer was then washed with NaHCO3, water and brine before being dried over Na2SO4 and concentrated under reduced pressure to yield an oil. The latter was partially purified by silica gel chromatography and then subjected to HPLC purification.

後処理

  1. customThe resulting reaction mixture
  2. customAfter removal of the solvent under reduced pressure
  3. additionthe resulting solid was poured into water
  4. extractionextracted twice with AcOEt
  5. washThe organic layer was then washed with NaHCO3, water and brine
  6. dry with materialbefore being dried over Na2SO4
  7. concentrationconcentrated under reduced pressure
  8. customto yield an oil
  9. customThe latter was partially purified by silica gel chromatography
  10. customsubjected to HPLC purification

出典と根拠

ORDレコード
ord-7fe0b12d0a7346b9ae8286c1b01efb0e
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08927533B2

反応ノート

読み込み中…

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