4-Toluenesulfonyl chloride → HCID 13362030、化合物

HRID 980952ノート

反応式

HRID 980952 の反応式
[CH2:1]([N:8]1[C:12](=[O:13])[CH2:11][CH:10]([CH2:14][OH:15])[CH:9]1[C:16]1[C:21]([Cl:22])=[CH:20][CH:19]=[CH:18][C:17]=1[Cl:23])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[S:24](Cl)([C:27]1[CH:33]=[CH:32][C:30]([CH3:31])=[CH:29][CH:28]=1)(=[O:26])=[O:25]>[K]>[CH2:1]([N:8]1[C:12](=[O:13])[CH2:11][CH:10]([CH2:14][O:15][S:24]([C:27]2[CH:33]=[CH:32][C:30]([CH3:31])=[CH:29][CH:28]=2)(=[O:26])=[O:25])[CH:9]1[C:16]1[C:17]([Cl:23])=[CH:18][CH:19]=[CH:20][C:21]=1[Cl:22])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 73974-Toluenesulfonyl chlorideHCID 13362029HCID 13362029、化合物

生成物 1

HCID 13362030HCID 13362030、化合物収率 77.2%

試薬・触媒・溶媒 1

HCID 5462222Potassium溶媒

実験手順

To 40 g of 1-benzyl-2-(2,6-dichlorophenyl)-3-hydroxymethyl-pyrrolidine-5-one in 67 ml of potassium dried pyridine at 5°-10° was added 23.3 g of tosyl chloride over 30 minutes. After the addition, the mixture was stirred for 3 hours at 15° and then for 13 hours at ambient temperature. The reaction mixture was added dropwise to a stirred ice-water solution and then set at ambient temperature for 72 hours. The light yellow solid was collected by filtration and then air dried. Trituration with ether followed by filtration provided 44.5 g of colorless crystals, m.p. 110°-114°.

後処理

  1. additionAfter the addition
  2. waitfor 13 hours at ambient temperature
  3. waitset at ambient temperature for 72 hours
  4. filtrationThe light yellow solid was collected by filtration
  5. customair dried
  6. filtrationTrituration with ether followed by filtration

出典と根拠

ORDレコード
ord-cb0c90902d7449b08e0389612e35ca27
出典データセット
uspto-grants-1987_01
特許番号
US04639529

反応ノート

読み込み中…