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Triethylamine → HCID 19068742, 화합물

HRID 1957242
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HRID 1957242 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[NH2:6][C:7]1[CH:8]=[C:9]([C:14]2[C:19]([Cl:20])=[CH:18][C:17]([C:21]([F:24])([F:23])[F:22])=[CH:16][N:15]=2)[CH:10]=[CH:11][C:12]=1[Cl:13].C(N(CC)CC)C>C(Cl)Cl>[Cl:20][C:19]1[C:14]([C:9]2[CH:10]=[CH:11][C:12]([Cl:13])=[C:7]([N:6]([S:2]([CH3:1])(=[O:4])=[O:3])[S:2]([CH3:1])(=[O:4])=[O:3])[CH:8]=2)=[N:15][CH:16]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 15766880HCID 15766880, 화합물

생성물 1

HCID 19068742HCID 19068742, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2.4 g (21.0 mmol) of methanesulfonyl chloride were slowly added dropwise to a mixture of 3.0 g (9.77 mmol) of 2-(3-amino-4-chlorophenyl)-3-chloro-5-trifluoromethylpyridine, 2.2 g (22.4 mmol) of triethylamine and 50 ml of anhydrous methylene chloride at 0°-5° C. The mixture was stirred at 20°-25° C. for about 15 hours and then washed twice with water, dried over sodium sulfate and finally concentrated. The residue was stirred with ether, filtered off with suction and dried under reduced pressure. Yield: 3.6 g (87%) of colorless crystals of melting point 230°-231° C.

후처리

  1. washwashed twice with water
  2. dry with materialdried over sodium sulfate
  3. concentrationfinally concentrated
  4. stirringThe residue was stirred with ether
  5. filtrationfiltered off with suction
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-8741899b6252463b9f91bc655a1d8a8f
출처 데이터셋
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05783522

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