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1,2-Dichloroethane → HCID 69936757、化合物

HRID 1623780
ノート
印刷プレビュー

反応式

HRID 1623780 の反応式
[CH:1]1[CH:2]=C[C:4]2[N:9](O)N=[N:7][C:5]=2[CH:6]=1.[CH3:11][N:12]([CH3:32])[C:13]([C:15]1[CH:16]=[CH:17][C:18]([O:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[C:19]([CH:23]=1)[C:20]([OH:22])=O)=[O:14].N1C=CC=C(N)C=1.C(Cl)CCl>CN(C)C=O.O>[CH3:32][N:12]([CH3:11])[C:13]([C:15]1[CH:16]=[CH:17][C:18]([O:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[C:19]([C:20]([NH:7][C:5]2[CH:4]=[N:9][CH:2]=[CH:1][CH:6]=2)=[O:22])[CH:23]=1)=[O:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 111,2-DichloroethaneHCID 100093-AminopyridineHCID 757711-HydroxybenzotriazoleHCID 67106993HCID 67106993、化合物

生成物 1

HCID 69936757HCID 69936757、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒

実験手順

HOBT (102 mg, 0.67 mmol) was added in one charge to a stirred solution of 5-[(dimethylamino)carbonyl]-2-[(phenylmethyl)oxy]benzoic acid (may be prepared as described in Description 59; 200 mg, 0.67 mmol), 3-pyridinamine (62.9 mg, 0.67 mmol) and EDC (128 mg, 0.67 mmol) in N,N-dimethylformamide (5 ml) under nitrogen at room temperature. The reaction mixture was stirred at room temperature for 4 h. The mixture was diluted with water (50 ml). The precipitate was collected by filtration. The solid was dissolved in ethyl acetate (100 ml), and the organic phase was washed with NaOH (1 mol/l 25 ml), water (25 ml), saturated brine (25 ml), dried over sodium sulfate, and evaporated in vacuo to yield the title compound as a white solid. 78 mg.

後処理

  1. filtrationThe precipitate was collected by filtration
  2. dissolutionThe solid was dissolved in ethyl acetate (100 ml)
  3. washthe organic phase was washed with NaOH (1 mol/l 25 ml), water (25 ml), saturated brine (25 ml)
  4. dry with materialdried over sodium sulfate
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-9d148bd02f994cab8908feea5236dd69
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08778939B2

反応ノート

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