Triethylamine → 5-(3-Methanesulfonylamino-propyl)-furan-2-carboxylic acid methyl ester

HRID 480364노트

반응식

HRID 480364 반응식
Cl.[CH3:2][O:3][C:4]([C:6]1[O:7][C:8]([CH2:11][CH2:12][CH2:13][NH2:14])=[CH:9][CH:10]=1)=[O:5].C(N(CC)CC)C.[CH3:22][S:23](Cl)(=[O:25])=[O:24]>C(Cl)Cl>[CH3:2][O:3][C:4]([C:6]1[O:7][C:8]([CH2:11][CH2:12][CH2:13][NH:14][S:23]([CH3:22])(=[O:25])=[O:24])=[CH:9][CH:10]=1)=[O:5]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chloride2회HCID 692922505-(3-Amino-propyl)-furan-2-carboxylic acid methyl ester hydrochloride salt

생성물 1

HCID 537273525-(3-Methanesulfonylamino-propyl)-furan-2-carboxylic acid methyl ester수율 87.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 5-(3-amino-propyl)-furan-2-carboxylic acid methyl ester hydrochloride salt (see Preparation DD2) (150 mg, 0.683 mmol), and triethylamine (0.313 mL, 2.25 mmol) in CH2Cl2 (15 mL) at 0° C. was added methanesulfonyl chloride (86 mg, 0.75 mmol) in CH2Cl2 (15 mL) at 0° C. was added methanesulfonyl chloride (86 mg, 0.75 was washed consecutively with dilute HCl, water, saturated NaHCO3, and brine. The organic solution was dried over MgSO4, filtered, and concentrated to provide the title sulfonamide (156 mg). MS 262 (M+1).

후처리

  1. washwas washed consecutively with dilute HCl, water, saturated NaHCO3, and brine
  2. dry with materialThe organic solution was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-fa3d93d8d99f4ed48918c9adba9de8e4
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06649657B2

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