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1,2-Dichloroethane → HCID 135525315、化合物

HRID 1455503
ノート
印刷プレビュー

反応式

HRID 1455503 の反応式
C(Cl)CCl.[Cl:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[NH:12][C:13]1[C:22]([C:23](O)=[O:24])=[CH:21][C:20]2[C:15](=[CH:16][C:17]([O:26]C)=[CH:18][CH:19]=2)[N:14]=1.[CH:28]1[CH:29]=[CH:30][C:31]2N(O)N=[N:34][C:32]=2[CH:33]=1.NC1C=CC=CC=1>CN(C=O)C.C(Cl)Cl>[C:32]1([NH:34][C:23]([C:22]2[C:13]([NH:12][C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=3[Cl:5])=[N:14][C:15]3[C:20]([CH:21]=2)=[CH:19][CH:18]=[C:17]([OH:26])[CH:16]=3)=[O:24])[CH:33]=[CH:28][CH:29]=[CH:30][CH:31]=1
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 6115AnilineHCID 757711-HydroxybenzotriazoleHCID 9858643HCID 9858643、化合物

生成物 1

HCID 135525315HCID 135525315、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

EDC (633 mg, 3.3 mmol) was added to a solution of 2-(2-Chloro-phenylamino)-7-methoxy-quinoline-3-carboxylic acid (986 mg, 3.0 mmol), HOBt (446 mg, 3.3 mmol) and aniline (307 mg, 3.3 mmol) in DMF (5 ml) at room temperature. After stirring the mixture for 1 hr, CH2Cl2 was used to extract the reaction mixture, and washed with water, saturated brine and then dried with magnesium sulfate. The solvent was removed under reduced pressure to give yellow oil. The yellow oil was purified by chromatography on SCX column using MeOH as eluent. At last, 2-(2-Chloro-phenylamino)-7-hydroxy-quinoline-3-carboxylic acid phenylamide was obtained as yellow solid after recrystallization from CH2Cl2 and Hexane; 947 mg (78%).

後処理

  1. extractionto extract the reaction mixture
  2. washwashed with water, saturated brine
  3. dry with materialdried with magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customto give yellow oil
  6. customThe yellow oil was purified by chromatography on SCX column

出典と根拠

ORDレコード
ord-00b0080823d042edb078e8ad7c6199fc
出典データセット
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07482455B2

反応ノート

読み込み中…

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