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Iodide Ion → HCID 22013732, 화합물

HRID 1532681
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HRID 1532681 반응식
[C:1]([O:5][CH2:6][CH3:7])(=[O:4])[CH:2]=O.[I-].[CH2:9]([NH:27][C:28]1[C:29]([NH2:34])=[CH:30][CH:31]=[CH:32][CH:33]=1)[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26].O.O.O.O.O.S([O-])([O-])(=O)=S.[Na+].[Na+]>C(O)C.O.C(OCC)(=O)C>[CH2:9]([N:27]1[C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=2[N:34]=[C:2]1[C:1]([O:5][CH2:6][CH3:7])=[O:4])[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 30165Iodide IonHCID 61475Sodium Thiosulfate PentahydrateHCID 70211Ethyl oxoacetateHCID 22013747HCID 22013747, 화합물

생성물 1

HCID 22013732HCID 22013732, 화합물수율 75.6%

시약·촉매·용매 3

HCID 702Ethanol용매
HCID 962
Water
용매
HCID 8857Ethyl Acetate용매

실험 절차

Ethyl glyoxylate (7.861 g) and iodide (4.886 g) were added to a solution containing N-octadecyl-1,2-benzenediamine (6.940 g) in ethanol (100 ml) and the mixture was stirred for 2 hours at room temperature. A solution containing sodium thiosulfate pentahydrate (4.813 g) in water (60 ml) was added dropwise to the reaction mixture while being stirred. The reaction mixture, with ethyl acetate added thereto, was washed with saturated brine, dried over sodium sulfate anhydride, and concentrated. The residue (10.06 g) was purified by silica gel column chromatography (silica gel 255 g, chloroform), thereby yielding the entitled compound (6.442 g) as pale yellow solid.

후처리

  1. additionwas added dropwise to the reaction mixture
  2. stirringwhile being stirred
  3. washwas washed with saturated brine
  4. dry with materialdried over sodium sulfate anhydride
  5. concentrationconcentrated
  6. customThe residue (10.06 g) was purified by silica gel column chromatography (silica gel 255 g, chloroform)

출처 및 근거

ORD 기록
ord-0ba52ffafd7c4794ae57e5f51340cd09
출처 데이터셋
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06204264B1

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