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Triethylamine hydrochloride → HCID 178442550、化合物

HRID 1653823
ノート
印刷プレビュー

反応式

HRID 1653823 の反応式
[C:1]1([C:7]2[N:8]=[C:9]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH:23]([CH3:26])[C:24]#[N:25])[O:10][C:11]=2[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N-:27]=[N+:28]=[N-:29].[Na+].Cl.C(N(CC)CC)C>CN(C)C=O>[C:1]1([C:7]2[N:8]=[C:9]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH:23]([C:24]3[NH:29][N:28]=[N:27][N:25]=3)[CH3:26])[O:10][C:11]=2[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
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 11130Triethylamine hydrochlorideHCID 33557Sodium AzideHCID 20080518HCID 20080518、化合物

生成物 1

HCID 178442550HCID 178442550、化合物収率 68.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3 g of (RS)-7(4,5-diphenyl-2-oxazolyl)-2-methylheptanenitrile in 30 cm3 of dimethylformamide are treated with twice 1.7 g of sodium azide and twice 3.6 g of triethylamine hydrochloride under the (time and temperature) conditions defined in Example 1. After treatment, the product of the reaction is chromatographed on a column 2 cm in diameter containing 78 g of silica gel (50 to 200μ). The column is eluted, collecting 200 cm3 fractions, with 1 liter of diisopropyl ether and then with 1.6 liters of a diisopropyl ether/ethyl acetate (95:5 by volume) mixture. The fractions from the last eluent mixture are concentrated to dryness under reduced pressure (0.2 kPa). 2.3 g (68%) of (RS)-5-[7-(4,5-diphenyl-2-oxazolyl)-2-heptyl]-1H-tetrazole are obtained in the form of a yellowish oil.

後処理

  1. customAfter treatment, the product of the reaction is chromatographed on a column 2 cm in diameter
  2. additioncontaining 78 g of silica gel (50 to 200μ)
  3. washThe column is eluted
  4. customcollecting 200 cm3 fractions
  5. concentrationThe fractions from the last eluent mixture are concentrated to dryness under reduced pressure (0.2 kPa)

出典と根拠

ORDレコード
ord-8165d3b2d32b47ff8317466058bab2cd
出典データセット
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05403852

反応ノート

読み込み中…

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