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

HRID 1776524노트

반응식

HRID 1776524 반응식
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

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 59443767HCID 59443767, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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]+).

후처리

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

출처 및 근거

ORD 기록
ord-6de8e336b2c44bb3a33d44674341c050
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09265768B2

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