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Diisopropylethylamine → HCID 69419383、化合物

HRID 1375085
ノート
印刷プレビュー

反応式

HRID 1375085 の反応式
[CH2:1]([O:3][C:4](=[O:22])[CH2:5][C:6]1([C:15]2[CH:20]=[CH:19][C:18]([NH2:21])=[CH:17][CH:16]=2)[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1)[CH3:2].[CH3:23][O:24][C:25]1[CH:26]=[C:27]([CH2:42][C:43](O)=[O:44])[CH:28]=[CH:29][C:30]=1[NH:31][C:32]([NH:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=1[CH3:41])=[O:33].C(N(C(C)C)CC)(C)C.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1>CN(C)C=O>[CH2:1]([O:3][C:4](=[O:22])[CH2:5][C:6]1([C:15]2[CH:20]=[CH:19][C:18]([NH:21][C:43](=[O:44])[CH2:42][C:27]3[CH:28]=[CH:29][C:30]([NH:31][C:32]([NH:34][C:35]4[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=4[CH3:41])=[O:33])=[C:25]([O:24][CH3:23])[CH:26]=3)=[CH:17][CH:16]=2)[CH2:7][C:8]2[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH2:14]1)[CH3:2]
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 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 114498403-Methoxy-4-o-tolylureidophenylacetic acidHCID 69419599[2-(4-Amino-phenyl)-indan-2-yl]-acetic Acid Ethyl Ester

生成物 1

HCID 69419383HCID 69419383、化合物収率 19%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

実験手順

A solution of [2-(4-amino-phenyl)-indan-2-yl]-acetic acid ethyl ester (0.158 g, Reference Example 10) in dimethylformamide (2 mL) was treated with a solution of [3-methoxy-4-(3-o-tolyl-ureido)-phenyl]-acetic acid (0.169 g) in dimethylformamide (2 mL) which had been treated with diisopropylethylamine (1.3 mL) and a solution of O-(7-azabenzotriazol-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate (0.223 g) in dimethylformamide (2 mL). After stirring at room temperature for 2 hours the reaction mixture was evaporated and the residue was partitioned between ethyl acetate (30 mL) and hydrochloric acid (30 mL, 0.5N). The organic phase was washed with hydrochloric acid (30 mL, 0.5N), then with saturated sodium hydrogen carbonate solution (30 mL), then dried over magnesium sulfate and then evaporated. The residual beige coloured solid was subjected to chromatography on silica eluting with a mixture of ethyl acetate and cyclohexane (2:1, v/v) to give the title compound (0.06 g).

後処理

  1. customwas evaporated
  2. customthe residue was partitioned between ethyl acetate (30 mL) and hydrochloric acid (30 mL, 0.5N)
  3. washThe organic phase was washed with hydrochloric acid (30 mL, 0.5N)
  4. dry with materialwith saturated sodium hydrogen carbonate solution (30 mL), then dried over magnesium sulfate
  5. customevaporated
  6. additionwas subjected to chromatography on silica eluting with a mixture of ethyl acetate and cyclohexane (2:1

出典と根拠

ORDレコード
ord-b0119a1b56204874adefe6de50e8ead5
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07166616B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート