HCID 89590802、化合物 → 1-(1-Hydroxy-1-methylethyl)cyclopropanesulfonamide

HRID 522356ノート

反応式

HRID 522356 の反応式
[OH:1][C:2]([C:5]1([S:8]([NH:11]C(=O)OCC2C=CC=CC=2)(=[O:10])=[O:9])[CH2:7][CH2:6]1)([CH3:4])[CH3:3]>CO.[Pd]>[OH:1][C:2]([C:5]1([S:8]([NH2:11])(=[O:9])=[O:10])[CH2:6][CH2:7]1)([CH3:4])[CH3:3]

参加物

4

反応物 1

HCID 89590802HCID 89590802、化合物

生成物 1

HCID 692665221-(1-Hydroxy-1-methylethyl)cyclopropanesulfonamide収率 68.7%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

To a solution of the product of Step 2 (995 mg) in methanol (30 mL) under nitrogen was added Pd/C (169 mg). The flask was purged with hydrogen and stirred for 3 hours. Celite was added to the reaction mixture and it was filtered through a pad of Celite. The solvent was removed in vacuo. The resulting residue was purified by flash chromatography (ISCO, 0 to 10% methanol in dichloromethane) to afford the desired product (391 mg). 1H NMR (400 MHz, CDCl3): δ (ppm) 4.88 (br s, 2H), 2.58 (s, 1H), 1.44-1.41 (m, 2H), 1.41 (s, 6H), 1.06-1.03 (m, 2H).

後処理

  1. customThe flask was purged with hydrogen
  2. additionCelite was added to the reaction mixture and it
  3. filtrationwas filtered through a pad of Celite
  4. customThe solvent was removed in vacuo
  5. customThe resulting residue was purified by flash chromatography (ISCO, 0 to 10% methanol in dichloromethane)

出典と根拠

ORDレコード
ord-fd70bef1fd0442bcbe0f70d16edc8730
出典データセット
uspto-grants-2016_05
特許番号
US09328138B2

反応ノート

読み込み中…