Iodine → Benzyl [2-(5-ethyloxazol-2-yl)ethyl]carbamate

HRID 1804554ノート

反応式

HRID 1804554 の反応式
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.II.C(N(CC)CC)C.O=[C:30]([CH2:48][CH3:49])[CH2:31][NH:32][C:33]([CH2:35][CH2:36][NH:37][C:38](=[O:47])[O:39][CH2:40][C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1)=[O:34]>ClCCl>[CH2:48]([C:30]1[O:34][C:33]([CH2:35][CH2:36][NH:37][C:38](=[O:47])[O:39][CH2:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)=[N:32][CH:31]=1)[CH3:49]

参加物

6

反応物 4

HCID 807IodineHCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 57637089Benzyl [2-(2-oxobutylcarbamoyl)ethyl]carbamate

生成物 1

HCID 57636953Benzyl [2-(5-ethyloxazol-2-yl)ethyl]carbamate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

23.07 g (49.60 mmol) PS-triphenylphosphine are suspended in 200 ml dichloromethane, 12.65 g (49.82 mmol) iodine are added. The mixture is stirred for 0.1 hours at ambient temperature, then 13.80 ml (99.28 mmol) triethylamine are added dropwise. 5.80 g (19.84 mmol) benzyl [2-(2-oxo-butylcarbamoyl)-ethyl]-carbamate dissolved in 150 ml dichloromethane are added. The reaction mixture is stirred for 72 hours at ambient temperature, then the precipitate is filtered off. The filtrate is extracted with water, the organic phase is dried and evaporated to dryness.

後処理

  1. additionare added
  2. stirringThe reaction mixture is stirred for 72 hours at ambient temperature
  3. filtrationthe precipitate is filtered off
  4. extractionThe filtrate is extracted with water
  5. customthe organic phase is dried
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-344c509a61b94b95b2a986106514681b
出典データセット
uspto-grants-2013_01
特許番号
US08354418B2

反応ノート

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