Sodium Carbonate → HCID 86699719、化合物

HRID 1844108ノート

反応式

HRID 1844108 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 86699719HCID 86699719、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-317dbfc389ca4de084b3ea04c288ea6c
出典データセット
uspto-grants-2015_02
特許番号
US08946282B2

反応ノート

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