Triphenylphosphine → HCID 21942891, 화합물

HRID 2216434노트

반응식

HRID 2216434 반응식
N(C(OC(C)C)=O)=NC(OC(C)C)=O.[C:15]([N:18]1[C:22]2[CH:23]=[CH:24][C:25]([Cl:27])=[CH:26][C:21]=2[S:20][CH:19]1[C:28]1[CH:33]=[C:32]([O:34][CH3:35])[CH:31]=[CH:30][C:29]=1[OH:36])(=[O:17])[CH3:16].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:56]1([CH3:71])[CH:61]=[CH:60][C:59]([S:62]([O:65][CH2:66][CH2:67][CH:68]([CH3:70])O)(=[O:64])=[O:63])=[CH:58][CH:57]=1>O1CCCC1>[C:15]([N:18]1[C:22]2[CH:23]=[CH:24][C:25]([Cl:27])=[CH:26][C:21]=2[S:20][CH:19]1[C:28]1[CH:33]=[C:32]([O:34][CH3:35])[CH:31]=[CH:30][C:29]=1[O:36][CH:68]([CH3:70])[CH2:67][CH2:66][O:65][S:62]([C:59]1[CH:58]=[CH:57][C:56]([CH3:71])=[CH:61][CH:60]=1)(=[O:63])=[O:64])(=[O:17])[CH3:16]

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 132043233-Hydroxybutyl 4-methylbenzenesulfonateHCID 14053536HCID 14053536, 화합물

생성물 1

HCID 21942891HCID 21942891, 화합물수율 37%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of diisopropyl azodicarboxylate (1.54 g, 7.61 mmol) in anhydrous tetrahydrofuran (10 ml) was added to a solution of 3-acetyl-6-chloro-2-(2-hydroxy-5-methoxyphenyl)benzothiazoline (2.56 g, 7.62 mmol), triphenylphosphine (2.00 g, 7.61 mmol) and 3-p-toluenesulfonyloxy-1-methylpropanol (1.86 g, 7.61 mmol) in anhydrous tetrahydrofuran (10 ml) at room temperature, and the mixture was stirred for four hours. The reaction mixture was concentrated, and the obtained oily matter was purified by silica gel column chromatography (mobile phase: hexane/ethyl acetate=4/1) to give 1.58 g (37%) of the target compound.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. customthe obtained oily matter was purified by silica gel column chromatography (mobile phase: hexane/ethyl acetate=4/1)

출처 및 근거

ORD 기록
ord-3c4d6cc6eff74ff0bb390b500ba26cf2
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07112598B2

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