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5-methyl-4-(methylamino)methyl-1-triphenylmethyl-1H-imidazole → HCID 19900737、化合物

HRID 1029512
ノート
印刷プレビュー

反応式

HRID 1029512 の反応式
[CH3:1][C:2]1[N:6]([C:7]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:5]=[N:4][C:3]=1[CH2:26][NH:27]C.[CH3:29][CH:30]1[CH2:39][CH2:38][C:37]2[C:32]3=[C:33]([C:40]([C:42]([OH:44])=O)=[CH:41][N:31]13)[CH:34]=[CH:35][CH:36]=2>C(#N)C>[CH3:1][C:2]1[N:6]([C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH:5]=[N:4][C:3]=1[CH2:26][NH:27][C:42]([C:40]1[C:33]2=[C:32]3[C:37](=[CH:36][CH:35]=[CH:34]2)[CH2:38][CH2:39][CH:30]([CH3:29])[N:31]3[CH:41]=1)=[O:44]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 153083055-methyl-4-(methylamino)methyl-1-triphenylmethyl-1H-imidazoleHCID 199007324-methyl-5,6-dihydro-4H-pyrrolo[3,2,1-ij]quinoline-1-carboxylic acid

生成物 1

HCID 19900737HCID 19900737、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 3.4 g (9.3 mmol) of 5-methyl-4-(methylamino) methyl-1-triphenylmethyl-1H-imidazole, 2.0 g (9.3 mmol) of 4-methyl-5,6-dihydro-4H-pyrrolo[3,2,1-ij]quinoline-1-carboxylic acid, and 2.06 g (10 mmol) of N,N-dicyclohexylcarbodiimide in 100 ml of acetonitrile was stirred for 12 hours under nitrogen. The precipitate was sucked off and the filtrate was evaporated in vacuo. The residue was dissolved in ethylacetate and washed with 2 N sodium hydroxide and saturated saline respectively, and then evaporated in vacuo. The residue was chromatographed on silicagel using methylene chloride/methanol (95/5) as an eluent. After evaporating the desired fractions 3.6 g of N-methyl, N-[(5-methyl-1-triphenylmethyl-1H-imidazol-4-yl)methyl]-4-methyl-5,6-dihydro-4H-pyrrolo[3,2,1-ij]quinoline-1-carboxamide were obtained.

後処理

  1. customthe filtrate was evaporated in vacuo
  2. dissolutionThe residue was dissolved in ethylacetate
  3. washwashed with 2 N sodium hydroxide and saturated saline respectively
  4. customevaporated in vacuo
  5. customThe residue was chromatographed on silicagel
  6. customAfter evaporating the desired fractions 3.6 g of N-methyl

出典と根拠

ORDレコード
ord-7ee14212a126443185592b0c574f4810
出典データセット
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05102901

反応ノート

読み込み中…

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