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Triethylamine → HCID 17912565, 화합물

HRID 963549
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HRID 963549 반응식
[F:1][C:2]([F:16])=[CH:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13](Cl)=[O:14].[CH2:17]([S:20]([C:23]1[CH:29]=[CH:28][C:26]([NH2:27])=[CH:25][CH:24]=1)(=[O:22])=[O:21])[CH2:18][CH3:19].C(N(CC)CC)C>CN(C)C1C=CN=CC=1.C1(C)C=CC=CC=1>[CH2:17]([S:20]([C:23]1[CH:24]=[CH:25][C:26]([NH:27][C:13](=[O:14])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH:3]=[C:2]([F:16])[F:1])=[CH:28][CH:29]=1)(=[O:22])=[O:21])[CH2:18][CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 5646714-(Propylsulfonyl)anilineHCID 14855873HCID 14855873, 화합물

생성물 1

HCID 17912565HCID 17912565, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 1140Toluene용매2회

실험 절차

8.5 g of 12,12-difluorododec-11-enoic acid chloride are added at room temperature to 3.45 g of 4-propylsulfonylaniline, 2.5 g of triethylamine and 100 mg of 4-dimethylaminopyridine in 50 ml of toluene and the mixture is stirred for 2 days at room temperature. A further 50 ml of toluene is then added, the toluene phase is washed with water, dried over sodium sulfate and concentrated to dryness by evaporation in vacuo. The residue is chromatographed on silica gel with hexane:ethyl acetate (7:3), yielding the title compound having a melting point of 67°-70° C. (compound no. 3-4).

후처리

  1. washthe toluene phase is washed with water
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated to dryness by evaporation in vacuo
  4. customThe residue is chromatographed on silica gel with hexane:ethyl acetate (7:3)

출처 및 근거

ORD 기록
ord-506aa05642c6492682b99828d2d99ce1
출처 데이터셋
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05763481

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