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Triethylamine → HCID 20552958, 화합물

HRID 1446822
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HRID 1446822 반응식
[NH2:1][C:2]1[CH:15]=[CH:14][CH:13]=[CH:12][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].[CH3:16][S:17][CH2:18][C:19]([NH:21][CH3:22])=[O:20].C(OCl)(C)(C)C.C(N(CC)CC)C>C(Cl)Cl>[NH2:1][C:2]1[C:3]([C:4](=[O:5])[C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)=[CH:12][CH:13]=[CH:14][C:15]=1[CH:18]([S:17][CH3:16])[C:19]([NH:21][CH3:22])=[O:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 760802-AminobenzophenoneHCID 521297Tert-Butyl hypochloriteHCID 13553138HCID 13553138, 화합물

생성물 1

HCID 20552958HCID 20552958, 화합물수율 65.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

A solution of 29.6 g (0.15 mole) of 2-aminobenzophenone in 350 ml of methylene chloride was cooled to -70° C. and 17.9 g (0.15 mol) of 2-methylthio-N-methylacetamide in 20 ml of methylene chloride was added. To the (-70° C.) mixture was added dropwise a solution of 17.2 g (0.15 mole) of 95% t-butylhypochlorite in 30 ml of methylene chloride. The temperature was maintained at or below -65° C. for 1.5 hr, then 15.1 g (0.15 mole) of triethylamine was added rapidly. The solution was allowed to warm to room temperature and was washed with water. The organic solution was concentrated and the residue crystallized when mixed with isopropyl ether. The solid was recrystallized from isopropyl alcohol to give 31 g (65%) of yellow needles, m.p. 149.0°-150.0° C.

후처리

  1. temperatureThe temperature was maintained at or below -65° C. for 1.5 hr
  2. washwas washed with water
  3. concentrationThe organic solution was concentrated
  4. customthe residue crystallized when
  5. additionmixed with isopropyl ether
  6. customThe solid was recrystallized from isopropyl alcohol

출처 및 근거

ORD 기록
ord-f43d5de94eaf463ebbd72af5054460ef
출처 데이터셋
uspto-grants-1982_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04313949

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