Sodium Carbonate → HCID 86699719, 화합물

HRID 1844108노트

반응식

HRID 1844108 반응식
ClC(OC(=O)OC(Cl)(Cl)Cl)(Cl)Cl.[CH3:13][N:14]1[CH2:18][CH2:17][N:16]([C:19](Cl)=[O:20])[C:15]1=[O:22].[NH2:23][C:24]1[CH:32]=[C:31]2[C:27]([CH2:28][C:29](=[O:33])[NH:30]2)=[CH:26][CH:25]=1.C(=O)([O-])[O-].[Na+].[Na+]>O1CCCC1>[CH3:13][N:14]1[CH2:18][CH2:17][N:16]([C:19]([NH:23][C:24]2[CH:32]=[C:31]3[C:27]([CH2:28][C:29](=[O:33])[NH:30]3)=[CH:26][CH:25]=2)=[O:20])[C:15]1=[O:22]

참가 물질

6

반응물 4

HCID 10340Sodium CarbonateHCID 94429TriphosgeneHCID 5905386-Amino-1,3-dihydro-2H-indol-2-oneHCID 205593403-Methyl-2-oxoimidazolidine-1-carbonyl chloride

생성물 1

HCID 86699719HCID 86699719, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

bis(trichloromethyl)carbonate in tetrahydrofuran was added dropwise within 1 hour to the compound D78 in tetrahydrofuran in such a way that the internal temperature was kept at 55-60° C. The mixture was stirred for 5 h at this temperature. The formation of 3-methyl-2-oxoimidazolidine-1-carbonyl chloride was confirmed by TLC. The 6-aminoindolin-2-one (D4) was added to the mixture in situ and the mixture was refluxed for 4 h. The completion of reaction was monitored using TLC. The residue obtained after workup using saturated sodium carbonate was further purified using flash chromatography on silica gel to afford the title compound D79.

후처리

  1. customwas kept at 55-60° C
  2. temperaturethe mixture was refluxed for 4 h
  3. customThe completion of reaction
  4. customThe residue obtained after workup
  5. customwas further purified

출처 및 근거

ORD 기록
ord-317dbfc389ca4de084b3ea04c288ea6c
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946282B2

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