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Triethylamine → 4-(2,4-dichlorophenyl)-5-methyl-2-[N-(dicyclopropylmethyl)-N-propylamino]thiazole

HRID 128696
ノート
印刷プレビュー

反応式

HRID 128696 の反応式
[CH:1]1([CH:4]([CH:12]2[CH2:14][CH2:13]2)[N:5]([CH2:9][CH2:10][CH3:11])[C:6]([NH2:8])=[S:7])[CH2:3][CH2:2]1.C(N(CC)CC)C.Br[CH:23]([CH3:34])[C:24]([C:26]1[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][C:27]=1[Cl:33])=O>C(O)C>[Cl:33][C:27]1[CH:28]=[C:29]([Cl:32])[CH:30]=[CH:31][C:26]=1[C:24]1[N:8]=[C:6]([N:5]([CH:4]([CH:1]2[CH2:3][CH2:2]2)[CH:12]2[CH2:13][CH2:14]2)[CH2:9][CH2:10][CH3:11])[S:7][C:23]=1[CH3:34]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 109239912-Bromo-1-(2,4-dichlorophenyl)propan-1-one2 回HCID 18967796N-(dicyclopropylmethyl)-N-propylthiourea2 回

生成物 1

HCID 193748924-(2,4-dichlorophenyl)-5-methyl-2-[N-(dicyclopropylmethyl)-N-propylamino]thiazole収率 88%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To 1 g of N-(dicyclopropylmethyl)-N-propylthiourea (Compound 88) dissolved in 25 ml of anhydrous ethanol, add 0.54 ml of triethylamine, then slowly 1 g of 2-bromo-1-(2,4-dichlorophenyl)-1-propanone (Compound 15). After two hours of heating under reflux of the ethanol, evaporate to dryness. Take up the residue in methylene chloride and wash with water until bromide ions have been removed completely. Dry the organic phase over anhydrous sodium sulphate and then evaporate to dryness. Purify the residue on a silica column, using a mixture of cyclohexane and ethyl acetate (20:1 V/V) as eluent, to obtain the expected product in the form of an oil.

後処理

  1. temperatureAfter two hours of heating
  2. customevaporate to dryness
  3. washwash with water until bromide ions
  4. customhave been removed completely
  5. dry with materialDry the organic phase over anhydrous sodium sulphate
  6. customevaporate to dryness
  7. customPurify the residue on a silica column
  8. additiona mixture of cyclohexane and ethyl acetate (20:1 V/V) as eluent

出典と根拠

ORDレコード
ord-ba9a4d120cfa490e85c15c7a62715150
出典データセット
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05464847

反応ノート

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