Ammonia → HCID 14391988、化合物

HRID 477112ノート

反応式

HRID 477112 の反応式
[F:1][C:2]([F:13])([F:12])[C:3]1[S:4][CH:5]=[C:6]([C:8](=[O:11])[CH2:9]Br)[N:7]=1.O[CH2:15][CH2:16][NH:17][CH:18]([CH3:32])[CH2:19][C:20]1[CH:25]=[CH:24][C:23]([O:26][CH2:27][C:28]([O:30][CH3:31])=[O:29])=[CH:22][CH:21]=1.C([SiH](CC)CC)C.N>>[C:28]([CH2:27][O:26][C:23]1[CH:24]=[CH:25][C:20]([CH2:19][CH:18]([N:17]2[CH2:16][CH2:15][O:11][CH:8]([C:6]3[N:7]=[C:3]([C:2]([F:13])([F:12])[F:1])[S:4][CH:5]=3)[CH2:9]2)[CH3:32])=[CH:21][CH:22]=1)([O:30][CH3:31])=[O:29]

参加物

5

反応物 4

HCID 222AmmoniaHCID 12052TriethylsilaneHCID 10978660HCID 10978660、化合物HCID 14347764HCID 14347764、化合物

生成物 1

HCID 14391988HCID 14391988、化合物

実験手順

Prepared analogously to Example 3 by reaction of 11.6 g (0.043 mol) of 2-trifluoromethyl-4-bromoacetyl-thiazole with 23 g (0.086 mol) of N-(2-hydroxyethyl)-2-(4-carbomethoxymethoxyphenyl)-1-methylethylamine. To complete the reaction the mixture is heated to boiling for 6 hours. It is then concentrated in vacuo, and the resulting residue is dissolved in 85 ml of trifluoroacetic acid and, at room temperature, 7 g (0.06 mol) of triethylsilane are added. After 90 hours the solution is poured onto ice, and concentrated ammonia is added, and the mixture is extracted several times with methylene chloride. The organic phase is dried over sodium sulphate and concentrated, and the residue is purified on a silica gel column using toluene/ethyl acetate=8/2 as eluant.

後処理

  1. customthe reaction the mixture
  2. temperatureis heated
  3. concentrationIt is then concentrated in vacuo
  4. dissolutionthe resulting residue is dissolved in 85 ml of trifluoroacetic acid and, at room temperature
  5. additionis added
  6. extractionthe mixture is extracted several times with methylene chloride
  7. dry with materialThe organic phase is dried over sodium sulphate
  8. concentrationconcentrated
  9. customthe residue is purified on a silica gel column

出典と根拠

ORDレコード
ord-cdcc39cd424e4135a7e4d534209425ea
出典データセット
uspto-grants-1989_12
特許番号
US04886814

反応ノート

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