Pyridine → HCID 53726966, 화합물

HRID 614009노트

반응식

HRID 614009 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[O:9][CH:8]([CH3:10])[CH2:7][C:6]2=[C:11]([NH2:13])[CH:12]=1.N1C=CC=CC=1.[CH2:20]([S:29](Cl)(=[O:31])=[O:30])[C:21]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)=[O:22]>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:12]=[C:11]([NH:13][S:29]([CH2:20][C:21]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[O:22])(=[O:31])=[O:30])[C:6]2[CH2:7][CH:8]([CH3:10])[O:9][C:5]=2[CH:4]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 122818442-Oxo-2-phenyl-ethanesulfonyl chlorideHCID 213298112,3-Dihydro-6-methoxy-2-methyl-4-benzofuranamine

생성물 1

HCID 53726966HCID 53726966, 화합물수율 51.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 15.5 grams of 2,3-dihydro-6-methoxy-2-methyl-4-benzofuranamine and 10.5 grams of anhydrous pyridine in 100 cc of methylene chloride cooled to 0°-5° C., a solution of 24.5 grams of phenacylsulfonyl chloride in 80 cc of methylene chloride is added. When the dripping is terminated the reaction mixture is warmed to room temperature and stirred for 5 hours. At the end of this time the solution is washed with water, dried over sodium sulfate and concentrated to dryness. Crystallization of the resulting thick oil from ethyl alcohol-ethyl ether gives 16 grams of the compound of the title which melts at 143°-145° C.

후처리

  1. customWhen the dripping is terminated the reaction mixture
  2. washAt the end of this time the solution is washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated to dryness
  5. customCrystallization of the resulting thick oil from ethyl alcohol-ethyl ether

출처 및 근거

ORD 기록
ord-5b737da5db70441ab59ff7293b24faf0
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04143055

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