Trifluoroacetic acid → HCID 178502740、化合物

HRID 271349ノート

反応式

HRID 271349 の反応式
C([O:5][C:6](=[O:18])[CH2:7][C@H:8]1[CH2:11][C@@H:10]([C:12](=[O:17])[N:13]([O:15][CH3:16])[CH3:14])[CH2:9]1)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[CH3:16][O:15][N:13]([CH3:14])[C:12]([C@@H:10]1[CH2:11][C@H:8]([CH2:7][C:6]([OH:18])=[O:5])[CH2:9]1)=[O:17]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 178502741HCID 178502741、化合物

生成物 1

HCID 178502740HCID 178502740、化合物収率 102.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To an ice cold solution of 2 g of cis-[3-(methoxy-methyl-carbamoyl)-cyclobutyl]-acetic acid tert-butyl ester in 25 mL of dichloromethane was added 10 mL of trifluoroacetic acid. The mixture was allowed to warm and stir for 2 h then concentrated under reduced pressure. The residue was taken up in 3×50 mL of toluene and repeatedly concentrated under reduced pressure to remove trifluoroacetic acid. Drying under vacuum overnight gave 1.6 g of product as a colorless oil: MS (m+1)=202.3; 1H NMR (400 MHz, CDCl3) 9.0 (br s, 1H), 3.62 (s, 3H), 3.18 (s, 3H), 2.65 (m, 1H), 2.5 (overlapping d and m, 3H), 2.4 (dd, 1H), 2.0 (, m, 2H).

後処理

  1. temperatureto warm
  2. concentrationthen concentrated under reduced pressure
  3. concentrationrepeatedly concentrated under reduced pressure
  4. customto remove trifluoroacetic acid
  5. customDrying under vacuum overnight

出典と根拠

ORDレコード
ord-860d91fe54e443459ff03a0de0adcc89
出典データセット
uspto-grants-2008_11
特許番号
US07452893B2

反応ノート

読み込み中…