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

HRID 480364ノート

反応式

HRID 480364 の反応式
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]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chloride2 回HCID 692922505-(3-Amino-propyl)-furan-2-carboxylic acid methyl ester hydrochloride salt

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-fa3d93d8d99f4ed48918c9adba9de8e4
出典データセット
uspto-grants-2003_11
特許番号
US06649657B2

反応ノート

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