Trifluoroacetic acid → HCID 69745714、化合物

HRID 1073014ノート

反応式

HRID 1073014 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-f18c5af6dc9647dc9fb388d75b3dd3f9
出典データセット
uspto-grants-2005_06
特許番号
US06911553B1

反応ノート

読み込み中…