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Triphenylphosphine → HCID 11539237, 화합물

HRID 1176717
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인쇄 미리보기

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HRID 1176717 반응식
O[C@H:2]1[CH2:7][C@@H:6]([CH3:8])[S:5](=[O:10])(=[O:9])[C:4]2[S:11][CH:12]=[CH:13][C:3]1=2.[CH2:14]([NH:16][S:17]([C:20]1[CH:25]=[CH:24][C:23]([N+:26]([O-:28])=[O:27])=[CH:22][CH:21]=1)(=[O:19])=[O:18])[CH3:15].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[OH-].[Na+]>C(Cl)Cl>[CH2:14]([N:16]([C@H:2]1[CH2:7][C@H:6]([CH3:8])[S:5](=[O:10])(=[O:9])[C:4]2[S:11][CH:12]=[CH:13][C:3]1=2)[S:17]([C:20]1[CH:21]=[CH:22][C:23]([N+:26]([O-:28])=[O:27])=[CH:24][CH:25]=1)(=[O:18])=[O:19])[CH3:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 14798Sodium HydroxideHCID 232621N-ethyl-4-nitrobenzenesulfonamideHCID 15647030HCID 15647030, 화합물

생성물 1

HCID 11539237HCID 11539237, 화합물수율 50.4%

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

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온도
-20 °C

실험 절차

Methylene chloride (60 mL), cis-4-hydroxy-5,6-dihydro-6-methyl-4-H-thieno-[2,3-b]-thiopyran-7,7-dioxide (5 g), N-ethyl-4-nitrobenzene-sulfonamide (6.86 g) and triphenyl-phosphine (8.42 g) are mixed under nitrogen atmosphere. The mixture is cooled to under −20° C. and diisopropyl azadicarboxylate (5.9 mL) is added, maintaining the temperature under −20° C. The temperature is allowed to rise to 20-25° C. The obtained mixture is treated with 5% NaOH (125 mL) and the resulting organic phase is vacuum distilled to dryness. The residue is chromatographed in a column (ethyl acetate/heptane, 2/1), obtaining 4.97 g of trans-4-[N-ethyl-N-(4-nitrobenzenesulfonyl)amino]-5,6-dihydro-6-methyl-4-H-thieno-[2,3-b]-thiopyran-7,7-dioxide.

후처리

  1. additionis added
  2. temperaturemaintaining the temperature under −20° C
  3. customto rise to 20-25° C
  4. distillationdistilled to dryness
  5. customThe residue is chromatographed in a column (ethyl acetate/heptane, 2/1)

출처 및 근거

ORD 기록
ord-4d200f30753241b8a8b2e083ffe991e8
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07842821B2

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