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Triethylamine → {1-[(1S)-1-(aminocarbonyl)propyl]-5-oxo-3-pyrrolidinyl}methyl 4-methylbenzenesulfonate

HRID 900310
ノート
印刷プレビュー

反応式

HRID 900310 の反応式
[OH:1][CH2:2][CH:3]1[CH2:7][N:6]([C@@H:8]([CH2:12][CH3:13])[C:9]([NH2:11])=[O:10])[C:5](=[O:14])[CH2:4]1.[CH2:15](N(CC)CC)C.[CH3:22][S:23](Cl)(=[O:25])=[O:24].N([CH2:30][CH:31]1[CH2:35]N([C@@H](CC)C(N)=O)[C:33](=O)[CH2:32]1)=[N+]=[N-]>C(Cl)Cl>[CH3:35][C:31]1[CH:30]=[CH:15][C:22]([S:23]([O:1][CH2:2][CH:3]2[CH2:4][C:5](=[O:14])[N:6]([C@H:8]([C:9]([NH2:11])=[O:10])[CH2:12][CH3:13])[CH2:7]2)(=[O:25])=[O:24])=[CH:33][CH:32]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471Triethylamine2 回HCID 31297Methanesulfonyl chloride2 回HCID 60105793(2S)-2-[4-(azidomethyl)-2-oxo-1-pyrrolidinyl]butanamideHCID 60105803(2S)-2-[4-(hydroxymethyl)2-oxo-1-pyrrolidinyl]butanamide

生成物 1

HCID 10291696{1-[(1S)-1-(aminocarbonyl)propyl]-5-oxo-3-pyrrolidinyl}methyl 4-methylbenzenesulfonate

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

In a 4 l three necked flask fitted with mechanical stirrer, dropping funnel and reflux condenser under inert atmosphere, 114 g (569 mmoles, 1 eq) of (2S)-2-[4-(hydroxymethyl)-2-oxo-1-pyrrolidinyl]butanamide 6 are dissolved in 2 l of CH2Cl2 and cooled down to 0° C. 158.5 ml (115 g, 2 eq) of dry triethylamine are added in one portion, followed by dropwise addition of a solution of 66.3 ml (96.2 g, 1.5 eq) of methanesulfonyl chloride in 190 ml of CH2Cl2 over 1 hour, all the while maintaining the temperature below 4° C. After 4 hours, 7.5 ml of methanesulfonyl chloride and 15 ml of triethylamine are added and the mixture is kept overnight in the refrigerator. The mixture is filtered, the residue washed with CH2Cl2 and the combined organic phases concentrated to dryness to give 216 g of crude 37. It is purified by Prep LC in several batches (1 kg SiO2, CH2Cl2/EtOH, 100:0->96:4) to give 109 g of pure 37, 69%. Alternatively, {1-[(1S)-1-(aminocarbonyl)propyl]-5-oxo-3-pyrrolidinyl}methyl 4-methylbenzenesulfonate 31 is prepared in an analogous way. 7.2.2. Synthesis of (2S)-2-[4-(azidomethyl)-2-oxo-1-pyrrolidinyl]butanamide 32

後処理

  1. temperatureall the while maintaining the temperature below 4° C
  2. waitthe mixture is kept overnight in the refrigerator
  3. filtrationThe mixture is filtered
  4. washthe residue washed with CH2Cl2
  5. concentrationthe combined organic phases concentrated to dryness
  6. customto give 216 g of crude 37
  7. customIt is purified by Prep LC in several batches (1 kg SiO2, CH2Cl2/EtOH, 100:0->96:4)
  8. customto give 109 g of pure 37, 69%

出典と根拠

ORDレコード
ord-32340ce2e42d4563bbdaf51e8f3f23ff
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07358276B2

反応ノート

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