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3-Methyl-2-butanone → HCID 71736007, 화합물

HRID 508290
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HRID 508290 반응식
[I:1][C:2]1[CH:3]=[C:4]([NH:9]N)[CH:5]=[C:6]([I:8])[CH:7]=1.[CH3:11][CH:12]([CH3:16])[C:13](=O)[CH3:14]>C(O)(=O)C>[I:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[C:4]2[C:3]=1[C:12]([CH3:16])([CH3:11])[C:13]([CH3:14])=[N:9]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 112513-Methyl-2-butanoneHCID 86695330HCID 86695330, 화합물

생성물 1

HCID 71736007HCID 71736007, 화합물수율 61.9%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

2 g of 3,5-diiodophenylhydrazine (5.5 mmol), and 1 mL (9.3 mmol) of 3-methyl-2-butanone were refluxed in 15 mL of acetic acid for 20 hours. The acetic acid was evaporated and the residue was dissolved in ether. Insoluble precipitate was filtered off, and the etheric solution was washed with aqueous solutions of NaHCO3, followed by Na2S2O3 and water. The organic layer was dried with CaCl2 and ether was removed under reduced pressure by a rotary evaporator to give 1.4 g of 4,6-diiodo-2,3,3-trimethyl-3H-indole. 1H-NMR (200 MHz, DMSO-d6), δ, ppm: 7.92 (1H, d, 1.1 Hz, arom.), 7.79 (1H, d, 1.1 Hz, arom.), 2.22 (3H, s, 2-CH3), 1.32 (6H, s, C(CH3)2).

후처리

  1. customThe acetic acid was evaporated
  2. dissolutionthe residue was dissolved in ether
  3. filtrationInsoluble precipitate was filtered off
  4. washthe etheric solution was washed with aqueous solutions of NaHCO3
  5. dry with materialThe organic layer was dried with CaCl2 and ether
  6. customwas removed under reduced pressure by a rotary evaporator

출처 및 근거

ORD 기록
ord-1813aada038d4d08a46b1abc5276f50c
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09095612B2

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