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m-Chloroperbenzoic acid → HCID 70287772, 화합물

HRID 850367
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HRID 850367 반응식
[CH2:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][CH:2]1[CH2:10][C:11]([N:13]1[C@H:17]([C:18]([N:20]2[CH2:24][CH2:23][CH2:22][CH2:21]2)=[O:19])[CH2:16][S:15][CH2:14]1)=[O:12].ClC1C=CC=C(C(OO)=[O:33])C=1>C(Cl)(Cl)Cl>[CH2:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][CH:2]1[CH2:10][C:11]([N:13]1[C@H:17]([C:18]([N:20]2[CH2:21][CH2:22][CH2:23][CH2:24]2)=[O:19])[CH2:16][S:15](=[O:33])[CH2:14]1)=[O:12]
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 9798234Z-321

생성물 1

HCID 70287772HCID 70287772, 화합물수율 73%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Dissolved in 100 ml of chloroform were 5 g of 3-(2-indanacetyl)-4(R)-(1-pyrrolidinecarbonyl)thiazolidine (a compound according to Preparation Example 2 set forth in Japanese Patent Application Laid-Open No. 262557/1990). While chilling with ice water, 3.3 g of meta-chloro-perbenzoic acid were gradually added to the solution. After stirring the mixture for 3 hours, the resultant liquid reaction mixture was washed successively with a 5% solution of sodium thiosulfate and a saturated aqueous solution of sodium bicarbonate and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by column chromatography on silica gel (methanol:chloroform=5:95), thereby obtaining 3.8 g of the title compound as a diastereomeric mixture. Yield: 73%.

후처리

  1. customaccording to Preparation Example 2
  2. additionwere gradually added to the solution
  3. customthe resultant liquid reaction mixture
  4. washwas washed successively with a 5% solution of sodium thiosulfate
  5. dry with materiala saturated aqueous solution of sodium bicarbonate and dried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off under reduced pressure
  7. customthe residue was purified by column chromatography on silica gel (methanol:chloroform=5:95)

출처 및 근거

ORD 기록
ord-dc38d8cd4eb146cca81276f4c7bc9ba8
출처 데이터셋
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06017929

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