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1,2-Dichloroethane → HCID 135525315, 화합물

HRID 1455503
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HRID 1455503 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 111,2-DichloroethaneHCID 6115AnilineHCID 757711-HydroxybenzotriazoleHCID 9858643HCID 9858643, 화합물

생성물 1

HCID 135525315HCID 135525315, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매
HCID 6344
Dichloromethane
용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-00b0080823d042edb078e8ad7c6199fc
출처 데이터셋
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07482455B2

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