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Dimethylformamide → HCID 3625286、化合物

HRID 2351823
ノート
印刷プレビュー

反応式

HRID 2351823 の反応式
C[N:2]([CH3:5])C=O.[CH2:6](N(CC)CC)C.[C:13](Cl)(=[O:17])[O:14]CC.Br[C:20]1[CH:21]=[CH:22][C:23]([O:26][C:27]2[CH:28]=[C:29]([CH:33]=[CH:34][CH:35]=2)[C:30](O)=O)=N[CH:25]=1>O1CCCC1>[O:26]([C:27]1[CH:28]=[C:29]([CH:33]=[CH:34][CH:35]=1)[CH2:30][CH:5]([C:13]([OH:17])=[O:14])[NH2:2])[C:23]1[CH:22]=[CH:21][CH:20]=[CH:25][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

6

反応物 4

HCID 6228DimethylformamideHCID 8471Triethylamine2 回HCID 10928Ethyl chloroformateHCID 198462343-(5-Bromo-2pyridyloxy)benzoic acid

生成物 1

HCID 3625286HCID 3625286、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

On the other hand, trans-4-(t-butoxycarbonyl)aminomethylcyclohexylcarbonxylic acid (1.62 g) was dissolved in dry tetrahydrofuran (50 ml) and dry N,N-dimethylformamide (20 ml), triethylamine (0.96 ml) was added to the resultant solution and a solution of ethyl chlorocarbonate (0.76 g) in tetrahydrofuran (2 ml) was added to the mixture under ice-cooling, followed by stirring for 30 minutes. To this solution was added the hydrochloride (III) previously obtained and triethylamine (2 ml) was added to the mixture, followed by stirring at room temperature for 3 hours. Ice-water (200 ml) was added to the reaction mixture and the precipitated crystalline substance was collected by filtration, thoroughly washed with water and dried to obtain 2.62 g of N-[trans-4(t-butyloxycarbonyl)aminomethylcyclohexylcarbonyl]-3-phenoxy-DL-phenylalanine 4-acetylanilide (IV) in the form of a white powder. The compound (IV) was confirmed by an NMR analysis.

後処理

  1. temperaturecooling
  2. custompreviously obtained
  3. stirringby stirring at room temperature for 3 hours
  4. filtrationthe precipitated crystalline substance was collected by filtration
  5. washthoroughly washed with water
  6. customdried

出典と根拠

ORDレコード
ord-443d958d57974a7aa7012cb0d2cf4354
出典データセット
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04873253

反応ノート

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