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Triethylamine → HCID 21273498、化合物

HRID 1382930
ノート
印刷プレビュー

反応式

HRID 1382930 の反応式
ClC(OCC(C)C)=O.[C:9]1([C:15]2[N:16]=[C:17]([CH2:26][CH2:27][C:28]([OH:30])=O)[NH:18][C:19]=2[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[CH2:31]([N:33](CC)CC)C.Cl.CN.N12CCCN=C1CCCCC2>CN(C)C=O.O>[CH3:31][NH:33][C:28](=[O:30])[CH2:27][CH2:26][C:17]1[NH:16][C:15]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)=[C:19]([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[N:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 8471Triethylamine2 回HCID 62365Isobutyl chloroformateHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 30431821H-Imidazole-2-propanoic acid, 4,5-diphenyl-HCID 6364545Methylamine hydrochloride

生成物 1

HCID 21273498HCID 21273498、化合物収率 65.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒2 回

実験手順

3.2 ml (0.024 mol) of isobutyl chloroformate are added dropwise at -5° to a solution of 7.0 g (0.024 mol) of 4,5-diphenylimidazole-2-propionic acid and 3.36 ml (0.024 mol) of triethylamine in 80 ml of dimethylformamide. After stirring at 0°-5° for 30 minutes 1.64 g (0.024 mol) of methylamine hydrochloride and 3.36 ml (0.024 mol) of triethylamine in 32 ml of dimethylformamide and 1.65 ml of water are added. The temperature is then left to rise to room temperature and the mixture is stirred for a further 20 hours. After concentration under reduced pressure the residue is boiled up in 250 ml of methanol and treated with 3.6 ml (0.024 mol) of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU), whereby a clear solution results. 4.8 g of N-methyl-4.5-diphenylimidazole-2-propionamide, m.p. 195°-200° (dec.), result by cooling in an ice-bath. From the mother liquor there are obtained by concentration and treatment with water a further 2 g of the same product, m.p. 195°-200°. Total yield: 6.8 g (93%).

後処理

  1. additionare added
  2. waitThe temperature is then left
  3. customto rise to room temperature
  4. concentrationAfter concentration under reduced pressure the residue
  5. customresults

出典と根拠

ORDレコード
ord-0f454b1c078c44f489bf330a73f1f2fd
出典データセット
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04808605

反応ノート

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