Water → HCID 70289093, 화합물

HRID 1872077노트

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HRID 1872077 반응식
[CH3:1][C:2]1[O:3][CH2:4][CH2:5][C:6]=1[C:7](Cl)=[O:8].[F:10][C:11]1[CH:17]=[CH:16][C:14](N)=[C:13](C2CCCCCCC2)[CH:12]=1.C([N:28]([CH2:31][CH3:32])[CH2:29][CH3:30])C.O>C1(C)C=CC=CC=1>[F:10][CH:11]1[CH2:12][CH2:13][CH2:14][CH2:16][CH2:32][CH:31]([N:28]([C:7]([C:6]2[CH2:5][CH2:4][O:3][C:2]=2[CH3:1])=[O:8])[C:29]2[CH:30]=[CH:5][CH:6]=[CH:2][CH:1]=2)[CH2:17]1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 117447752-methyl-4,5-dihydrofuran-3-carbonyl ChlorideHCID 15376472HCID 15376472, 화합물

생성물 1

HCID 70289093HCID 70289093, 화합물수율 132.8%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

At room temperature, a solution of 1.5 g (0.01 mol) of 2-methyl-4,5-dihydrofuran-3-carbonyl chloride in 10 ml of toluene is added dropwise with stirring to a mixture of 2.2 g (0.01 mol) of 4-fluoro-2-cyclooctylaniline, 1.0 g of triethylamine and 40 ml of toluene. After the addition has ended, the reaction mixture is stirred at room temperature for another 2 hours. The reaction mixture is subsequently admixed with water. The organic phase is separated off, dried over sodium sulphate and then concentrated under reduced pressure. The residue that remains is stirred with hexane. The resulting crystalline product is filtered off with suction and dried at 50° C. under reduced pressure. In this manner, 2.2 g (66.7% of theory) of N-(4-fluoro-2-cyclooctyl)-2-methyl-4,5-dihydrofuran-3-carboxanilide are obtained in the form of a solid substance of melting point 91° C.

후처리

  1. additionAfter the addition
  2. customThe organic phase is separated off
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated under reduced pressure
  5. stirringThe residue that remains is stirred with hexane
  6. filtrationThe resulting crystalline product is filtered off with suction
  7. customdried at 50° C. under reduced pressure

출처 및 근거

ORD 기록
ord-be5437be0f9f4ff282a9bf959d856081
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06107336

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