Water → 3,5-dimethyl-4-([1,4]oxazepane-4-sulfonyl)-1H-pyrrole-2-carboxylic acid ethyl ester

HRID 2375805ノート

反応式

HRID 2375805 の反応式
Cl.[O:2]1[CH2:8][CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.CCN(C(C)C)C(C)C.[CH2:18]([O:20][C:21]([C:23]1[NH:24][C:25]([CH3:33])=[C:26]([S:29](Cl)(=[O:31])=[O:30])[C:27]=1[CH3:28])=[O:22])[CH3:19].O>C(Cl)Cl>[CH2:18]([O:20][C:21]([C:23]1[NH:24][C:25]([CH3:33])=[C:26]([S:29]([N:5]2[CH2:6][CH2:7][CH2:8][O:2][CH2:3][CH2:4]2)(=[O:30])=[O:31])[C:27]=1[CH3:28])=[O:22])[CH3:19]

参加物

6

反応物 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 2776544ethyl 4-(chlorosulfonyl)-3,5-dimethyl-1H-pyrrole-2-carboxylateHCID 230902141,4-Oxazepane hydrochloride

生成物 1

HCID 692881593,5-dimethyl-4-([1,4]oxazepane-4-sulfonyl)-1H-pyrrole-2-carboxylic acid ethyl ester収率 101%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To [1,4]oxazepane hydrochloride (400 mg) in DCM (45 mL) was added DIEA (2.70 mL) followed by 4-chlorosulfonyl-3,5-dimethyl-1H-pyrrole-2-carboxylic acid ethyl ester (1.05 g). The mixture was stirred for 1 h at RT after which water was added and the resulting two phases were separated. The organic phase was washed two times with saturated aqueous NaHCO3 solution, dried over MgSO4 and concentrated to give crude) 3,5-dimethyl-4-([1,4]oxazepane-4-sulfonyl)-1H-pyrrole-2-carboxylic acid ethyl ester (970 mg) which was used directly in the following step.

後処理

  1. additionwas added
  2. customthe resulting two phases were separated
  3. washThe organic phase was washed two times with saturated aqueous NaHCO3 solution
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-e88dcafadfa04c56af0a42dc2674c4ef
出典データセット
uspto-grants-2008_12
特許番号
US07465806B2

反応ノート

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