Triethylamine → [1-[(Phenylmethyl)sulfonyl]-3-pyrrolidinyl]-carbamic acid, 1,1-dimethylethyl ester

HRID 38261

反応式

HRID 38261 の反応式
[NH:1]1[CH2:5][CH2:4][CH:3]([NH:6][C:7](=[O:13])[O:8][C:9]([CH3:12])([CH3:11])[CH3:10])[CH2:2]1.C(N(CC)CC)C.[CH:21]1[CH:26]=[CH:25][C:24]([CH2:27][S:28](Cl)(=[O:30])=[O:29])=[CH:23][CH:22]=1>ClCCl>[C:24]1([CH2:27][S:28]([N:1]2[CH2:5][CH2:4][CH:3]([NH:6][C:7](=[O:13])[O:8][C:9]([CH3:10])([CH3:12])[CH3:11])[CH2:2]2)(=[O:30])=[O:29])[CH:25]=[CH:26][CH:21]=[CH:22][CH:23]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 74740Phenylmethanesulfonyl chlorideHCID 2757234tert-butyl N-(pyrrolidin-3-yl)carbamate

生成物 1

HCID 91332323[1-[(Phenylmethyl)sulfonyl]-3-pyrrolidinyl]-carbamic acid, 1,1-dimethylethyl ester収率 65.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

To a solution/suspension of 3-pyrrolidinyl-carbamic acid, 1,1-dimethylethyl ester (0.5 g) and triethylamine (0.38 ml) in dichloromethane (30 ml) at 0° C. was added benzenemethanesulfonyl chloride (0.51 g). The mixture was stirred at 0° C. for 30 minutes then stirred at room temperature for 2 days. The reaction was diluted with dichloromethane (20 ml) washed with water, saturated aq. NaHCO3(aq), dried (MgSO4) and concentrated in vacuo to give the sub-title compound (0.6 g).

後処理

  1. stirringthen stirred at room temperature for 2 days
  2. washwashed with water, saturated aq. NaHCO3(aq)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-dbe3b2d374234cb39ea5c3d57766ebce
出典データセット
uspto-grants-2013_09
特許番号
US08524715B2

関連ノート

読み込み中…