4-Toluenesulfonyl chloride → HCID 13362030, 화합물

HRID 1632627노트

반응식

HRID 1632627 반응식
[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

참가 물질

4

반응물 2

HCID 73974-Toluenesulfonyl chlorideHCID 13362029HCID 13362029, 화합물

생성물 1

HCID 13362030HCID 13362030, 화합물수율 77.2%

시약·촉매·용매 1

HCID 5462222Potassium용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-d47fce4198fa4649acfe2b45cc1eb6bc
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04476311

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