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Triphenylphosphine → 4-[4-(p-Chlorophenylsulfonamido)butyl)-epsilon-caprolactone

HRID 465554
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인쇄 미리보기

반응식

HRID 465554 반응식
O[CH2:2][CH2:3][CH2:4][CH2:5][CH:6]1[CH2:13][CH2:12][O:11][C:9](=[O:10])[CH2:8][CH2:7]1.[Cl:14][C:15]1[CH:20]=[CH:19][C:18]([S:21]([NH2:24])(=[O:23])=[O:22])=[CH:17][CH:16]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>C(Cl)Cl.O1CCCC1>[Cl:14][C:15]1[CH:16]=[CH:17][C:18]([S:21]([NH:24][CH2:2][CH2:3][CH2:4][CH2:5][CH:6]2[CH2:13][CH2:12][O:11][C:9](=[O:10])[CH2:8][CH2:7]2)(=[O:22])=[O:23])=[CH:19][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 11776TriphenylphosphineHCID 668244-ChlorobenzenesulfonamideHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 103300695-(4-Hydroxybutyl)oxepan-2-one

생성물 1

HCID 103611324-[4-(p-Chlorophenylsulfonamido)butyl)-epsilon-caprolactone

시약·촉매·용매 2

HCID 6344
Dichloromethane
용매
HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 3.53 g of 4-(4-hydroxybutyl)-epsilon-caprolactone in 14 ml methylene chloride and 14 ml tetrahydrofuran is added 4.24 g p-chlorophenylsulfonamide followed by 7.44 g triphenylphosphine. The reaction mixture is stirred at room temperature for 0.5 h and then 6.1 ml diethyl azodicarboxylate is added slowly with cooling. After the addition, the cooling bath is removed and the solution is stirred at room temperature overnight. The reaction mixture is evaporated to dryness to yield 4-[4-(p-chlorophenylsulfonamido)butyl)-epsilon-caprolactone.

후처리

  1. temperaturewith cooling
  2. additionAfter the addition
  3. customthe cooling bath is removed
  4. stirringthe solution is stirred at room temperature overnight
  5. customThe reaction mixture is evaporated to dryness

출처 및 근거

ORD 기록
ord-82aaf2a46a714d7e8ebfb5170c20d777
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05153214

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