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Ammonium Chloride → HCID 69422773、化合物

HRID 349992
ノート
印刷プレビュー

反応式

HRID 349992 の反応式
C1(C)C=CC(S([CH2:10][N+:11]#[C-])(=O)=O)=CC=1.CC(C)([O-])C.[K+].[CH2:20]([O:27][C:28]1[CH:48]=[CH:47][C:31]([CH2:32][N:33]2[CH:37]=[C:36]([CH:38]=O)[C:35]([C:40]3[CH:45]=[CH:44][C:43]([F:46])=[CH:42][CH:41]=3)=[N:34]2)=[CH:30][CH:29]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[Cl-].[NH4+]>C(COC)OC.CO>[CH2:20]([O:27][C:28]1[CH:48]=[CH:47][C:31]([CH2:32][N:33]2[CH:37]=[C:36]([CH2:38][C:10]#[N:11])[C:35]([C:40]3[CH:45]=[CH:44][C:43]([F:46])=[CH:42][CH:41]=3)=[N:34]2)=[CH:30][CH:29]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 25517Ammonium ChlorideHCID 161915Tosylmethyl isocyanideHCID 23025043HCID 23025043、化合物HCID 23665647Potassium tert-butoxide

生成物 1

HCID 69422773HCID 69422773、化合物収率 76%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 8071
1,2-Dimethoxyethane
溶媒
3 回

実験手順

A solution of p-toluenesulfonylmethylisocyanide (3.08 g) in dimethoxyethane (15 ml) was added to a mixture of potassium t-butoxide (3.37 g) and dimethoxyethane (15 ml) at −78° C., and the resultant was stirred for 5 minutes. A solution of 1-(4-benzyloxybenzyl)-3-(4-fluorophenyl)-1H-pyrazole-4-carbaldehyde (5.80 g) in dimethoxyethane (30 ml) was added to the mixture. After stirring at the same temperature, the mixture was stirred for 1 hour while raising the temperature. Methanol (45 ml) was added to the mixture, which was refluxed for 1 hour. After cooling, the reaction mixture was poured into saturated aqueous ammonium chloride solution, which was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous sodium chloride solution, dried (MgSO4), and concentrated. The residue was subjected to silica gel column chromatography to obtain 1-(4-benzyloxybenzyl)-3-(4-fluorophenyl)-1H-pyrazol-4-ylacetonitrile (4.52 g, yield 76%) as colorless crystals from the fraction eluted with ethyl acetate-hexane (1:2, volume ratio). This was recrystallized from ethyl acetate-hexane. Melting point: 86–87° C.

後処理

  1. stirringAfter stirring at the same temperature
  2. stirringthe mixture was stirred for 1 hour
  3. temperaturewhile raising the temperature
  4. temperaturewas refluxed for 1 hour
  5. temperatureAfter cooling
  6. extractionwas extracted with ethyl acetate
  7. washThe ethyl acetate layer was washed with saturated aqueous sodium chloride solution
  8. dry with materialdried (MgSO4)
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-1ecd2f870cdf47258ddedd4122eecc76
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07179823B1

反応ノート

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