Trifluoroacetic acid → HCID 69745714、化合物

HRID 1530860ノート

反応式

HRID 1530860 の反応式
FC(F)(F)C(O)=O.[Si:8]([O:25][CH:26]([CH2:48][O:49]C(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[CH2:27][O:28][C:29](=[O:47])[CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36]/[CH:37]=[CH:38]\[CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH3:46])([C:21]([CH3:24])([CH3:23])[CH3:22])([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>ClCCl>[Si:8]([O:25][CH:26]([CH2:48][OH:49])[CH2:27][O:28][C:29](=[O:47])[CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36]/[CH:37]=[CH:38]\[CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH3:46])([C:21]([CH3:22])([CH3:24])[CH3:23])([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 69746545HCID 69746545、化合物

生成物 1

HCID 69745714HCID 69745714、化合物収率 54%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

4 ml of trifluoroacetic acid is slowly dropped into a solution of 4 (4.65 mmol) in 50 ml of dichloromethane at room temperature. After 3 hours, this is washed with water and saturated sodium hydrogen carbonate solution. The combined organic phases are dried over MgSO4, filtrated and concentrated. The residue is purified on silica gel by flash chromatography using isohexane/ethyl acetate (7:1). Yield: 54% of a colorless oil.

後処理

  1. washthis is washed with water and saturated sodium hydrogen carbonate solution
  2. dry with materialThe combined organic phases are dried over MgSO4
  3. filtrationfiltrated
  4. concentrationconcentrated
  5. customThe residue is purified on silica gel by flash chromatography

出典と根拠

ORDレコード
ord-8f280ca814d04ff38eb9c2d1e14bb474
出典データセット
uspto-grants-2001_03
特許番号
US06197759B1

反応ノート

読み込み中…