HCID 59457665、化合物 → HCID 59457731、化合物

HRID 1711096ノート

反応式

HRID 1711096 の反応式
[F:1][C:2]1[CH:30]=[C:29]([N+:31]([O-:33])=[O:32])[CH:28]=[CH:27][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]2[CH:11]=[C:12]([C:14]3[CH2:19][CH2:18][N:17](C(OC(C)(C)C)=O)[CH2:16][CH:15]=3)[S:13][C:6]=12>C(Cl)Cl>[F:1][C:2]1[CH:30]=[C:29]([N+:31]([O-:33])=[O:32])[CH:28]=[CH:27][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]2[CH:11]=[C:12]([C:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH:15]=3)[S:13][C:6]=12

参加物

3

反応物 1

HCID 59457665HCID 59457665、化合物

生成物 1

HCID 59457731HCID 59457731、化合物収率 101.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of the carboxylate 388 (1 g, 2.13 mmol) in DCM (4.3 mL) TFA (4.3 mL) was added and the reaction mixture was stirred 2 h at room temperature. The solvent was removed under reduced pressure, the residue was suspended in aqueous sodium bicarbonate, the mixture was extracted with DCM, EtOAc and DCM; the combined extracts were filtered and the recovered solids were collected and dried. The filtrate was dried over anhydrous Na2SO4, concentrated under reduced pressure and the residue was combined with the solid material obtained upon filtration, to afford 389 (806 mg, 100% yield) as a yellow solid. LCMS:(M+H) 372.1.

後処理

  1. customThe solvent was removed under reduced pressure
  2. extractionthe mixture was extracted with DCM, EtOAc and DCM
  3. filtrationthe combined extracts were filtered
  4. customthe recovered solids were collected
  5. customdried
  6. dry with materialThe filtrate was dried over anhydrous Na2SO4
  7. concentrationconcentrated under reduced pressure
  8. customobtained upon filtration

出典と根拠

ORDレコード
ord-1db1c13ae1de406dbb8a411222b51d45
出典データセット
uspto-grants-2010_09
特許番号
US07790729B2

反応ノート

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