Acetoxyacetyl chloride → HCID 59824354, 화합물

HRID 1645490

반응식

HRID 1645490 반응식
[CH2:1]([N:4]([CH3:20])[C:5]([C:7]1[C:8]([I:19])=[C:9]([C:13]([I:18])=[C:14]([NH2:17])[C:15]=1[I:16])[C:10]([Cl:12])=[O:11])=[O:6])[CH:2]=[CH2:3].[C:21]([O:24][CH2:25][C:26](Cl)=[O:27])(=[O:23])[CH3:22]>CC(N(C)C)=O>[CH2:1]([N:4]([CH3:20])[C:5]([C:7]1[C:15]([I:16])=[C:14]([NH:17][C:26]([CH2:25][O:24][C:21](=[O:23])[CH3:22])=[O:27])[C:13]([I:18])=[C:9]([C:10]([Cl:12])=[O:11])[C:8]=1[I:19])=[O:6])[CH:2]=[CH2:3]

참가 물질

4

반응물 2

HCID 26297Acetoxyacetyl chlorideHCID 598243643-(Allyl-methyl-carbamoyl)-5-amino-2,4,6-triiodo-benzoyl chloride

생성물 1

HCID 59824354HCID 59824354, 화합물수율 91%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

3-(Allyl-methyl-carbamoyl)-5-amino-2,4,6-triiodo-benzoyl chloride (8) (5 g, 7.93 mmol) was dissolved in dry DMA (20 mL) was acetoxyacetyl chloride (1.7 mL, 15.9 mmol) was added dropwise. The reaction mixture was stirred at overnight at RT, with nitrogen bubbling through the reaction mixture. The reaction was monitored by TLC on silica gel plates eluting with ethyl acetate: petrol (1:1). (6) had an Rf of 0.62 and 0.76 whilst there were two new spots at 0.32 and 0.22. The solution was diluted with ethyl acetate (˜100 mL) and washed with ice water/brine (50:50, 20 ml×5). The organics were dried over MgSO4, filtered, concentrated and dried under high vacuum to give the desired compound (5.26 g, 91%). The structure was confirmed by 1H and 13C NMR, and purity by LCMS.

후처리

  1. additionwas added dropwise
  2. washeluting with ethyl acetate: petrol (1:1)
  3. additionThe solution was diluted with ethyl acetate (˜100 mL)
  4. washwashed with ice water/brine (50:50, 20 ml×5)
  5. dry with materialThe organics were dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customdried under high vacuum

출처 및 근거

ORD 기록
ord-8d6405662a994c9d8c17afa5f36a0346
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08124806B2

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