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Water → 3-(2,6-Dichloroanilino)-2-thiophenglyoxylic acid ethyl ester

HRID 1680161
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반응식

HRID 1680161 반응식
[Cl:1][C:2]1[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[C:3]=1[NH:4][C:5]1[CH:9]=[CH:8][S:7][CH:6]=1.C(N(CC)CC)C.[CH2:22]([O:24][C:25](=[O:29])[C:26](Cl)=[O:27])[CH3:23].O>O1CCCC1.C(OCC)(=O)C>[CH2:22]([O:24][C:25](=[O:29])[C:26]([C:6]1[S:7][CH:8]=[CH:9][C:5]=1[NH:4][C:3]1[C:10]([Cl:14])=[CH:11][CH:12]=[CH:13][C:2]=1[Cl:1])=[O:27])[CH3:23]
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참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 20884Ethoxalyl chlorideHCID 234572233-(2,6-Dichloroanilino)thiophen

생성물 1

HCID 705760593-(2,6-Dichloroanilino)-2-thiophenglyoxylic acid ethyl ester

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매
HCID 8857
Ethyl Acetate
용매

실험 절차

2.44 g (10 mmoles) of 3-(2,6-dichloroanilino)thiophen, 1.01 g of triethylamine and 1.37 g (10 mmoles) of chlorooxalic acid ethyl ester are stirred in 20 ml of tetrahydrofuran at room temperature for 10 hours. 100 ml each of water and ethyl acetate are added, and the organic phase is dried and concentrated. Recrystallization of the residue from ethanol gives 3-(2,6-dichloroanilino)-2-thiophenglyoxylic acid ethyl ester.

후처리

  1. customthe organic phase is dried
  2. concentrationconcentrated
  3. customRecrystallization of the residue from ethanol

출처 및 근거

ORD 기록
ord-82acdef777024c0cbb806856f3439b3d
출처 데이터셋
uspto-grants-1981_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04272507

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