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Pyridine → 3-n-Butyl-5-(4-cyanobenzyl) hydantoin

HRID 847726
ノート
印刷プレビュー

反応式

HRID 847726 の反応式
FC(F)(F)C([NH:5]OC(=O)C(F)(F)F)=O.N1C=CC=CC=1.[CH2:21]([N:25]1[C:29](=[O:30])[CH:28]([CH2:31][C:32]2[CH:37]=[CH:36][C:35]([CH:38]=O)=[CH:34][CH:33]=2)[NH:27][C:26]1=[O:40])[CH2:22][CH2:23][CH3:24]>C1C=CC=CC=1>[CH2:21]([N:25]1[C:29](=[O:30])[CH:28]([CH2:31][C:32]2[CH:37]=[CH:36][C:35]([C:38]#[N:5])=[CH:34][CH:33]=2)[NH:27][C:26]1=[O:40])[CH2:22][CH2:23][CH3:24]
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 1049PyridineHCID 69634(2,2,2-Trifluoroacetyl)azanyl 2,2,2-trifluoroacetateHCID 127907213-n-Butyl-5-(4-formylbenzyl) hydantoin

生成物 1

HCID 127907633-n-Butyl-5-(4-cyanobenzyl) hydantoin

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

The formyl compound (4.3 g., 0.01 mole), N,O-bis (trifluoroacetyl)hydroxylamine (3.6 g., 0.016 mole) and dry pyridine (2.6 ml. 0.032 mole) were mixed in benzene (75 ml) and heated under reflux for 2 hours. After cooling the benzene solution was washed with water (2×50 ml), dried over magnesium sulphate monohydrate and evaporated in vacuo to give an oil which slowly crystallised. This product was further purified by silica gel chromatography and recrystallisation from a small volume of ethyl acetate to give the title compound, yield 2.5 g., m.p. 136° C.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 2 hours
  3. washwas washed with water (2×50 ml)
  4. dry with materialdried over magnesium sulphate monohydrate
  5. customevaporated in vacuo
  6. customto give an oil which
  7. customslowly crystallised
  8. customThis product was further purified by silica gel chromatography and recrystallisation from a small volume of ethyl acetate

出典と根拠

ORDレコード
ord-5572030541d544d6852e666020d13bb4
出典データセット
uspto-grants-1981_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04293563

反応ノート

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