Hydrochloric Acid → Methyl 3-(cyclopropylmethoxy)-4-(methylsulfonamido)benzoate

HRID 1776524ノート

反応式

HRID 1776524 の反応式
C(OC([N:8]([C:13]1[CH:22]=[CH:21][C:16]([C:17]([O:19][CH3:20])=[O:18])=[CH:15][C:14]=1[O:23][CH2:24][CH:25]1[CH2:27][CH2:26]1)[S:9]([CH3:12])(=[O:11])=[O:10])=O)(C)(C)C.Cl.O1CCOCC1>C(Cl)Cl>[CH:25]1([CH2:24][O:23][C:14]2[CH:15]=[C:16]([CH:21]=[CH:22][C:13]=2[NH:8][S:9]([CH3:12])(=[O:11])=[O:10])[C:17]([O:19][CH3:20])=[O:18])[CH2:26][CH2:27]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 59443767HCID 59443767、化合物

生成物 1

HCID 59443764Methyl 3-(cyclopropylmethoxy)-4-(methylsulfonamido)benzoate収率 96%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of methyl 4-(N-(tert-butoxycarbonyl)methylsulfonamido)-3-(cyclopropylmethoxy)benzoate (for reference procedure see Example 18, WO 2010/089107, which is incorporated herein by reference) (3.00 g, 7.51 mmol) in dry DCM (40 ml), HCl 4M in Dioxane (9.39 ml, 37.6 mmol) was added, and the mixture was stirred at RT for 3 days. The solvent was evaporated, the residue was triturated with iPr2O (50 ml) and filtered to give methyl 3-(cyclopropylmethoxy)-4-(methylsulfonamido)benzoate as an off-white powder (2.15 g, 7.18 mmol, 96% yield, MS/ESI+ 299.9 [MH]+).

後処理

  1. customThe solvent was evaporated
  2. customthe residue was triturated with iPr2O (50 ml)
  3. filtrationfiltered

出典と根拠

ORDレコード
ord-6de8e336b2c44bb3a33d44674341c050
出典データセット
uspto-grants-2016_02
特許番号
US09265768B2

反応ノート

読み込み中…