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1,2-Dichloroethane → HCID 60061360, 화합물

HRID 1839832
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HRID 1839832 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:16]=[CH:15][CH:14]=[C:13]3[C:9]=2/[C:10](=[CH:18]/[C:19]2[NH:20][C:21]([CH3:27])=[CH:22][C:23]=2[C:24](O)=[O:25])/[C:11](=[O:17])[NH:12]3)[CH:5]=[CH:6][CH:7]=1.C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl.[F:42][C:43]([F:50])([F:49])[CH2:44][NH:45][CH2:46][CH2:47][NH2:48]>CN(C=O)C>[F:42][C:43]([F:50])([F:49])[CH2:44][NH:45][CH2:46][CH2:47][NH:48][C:24]([C:23]1[CH:22]=[C:21]([CH3:27])[NH:20][C:19]=1/[CH:18]=[C:10]1\[C:11](=[O:17])[NH:12][C:13]2[C:9]\1=[C:8]([C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[CH:3]=1)[CH:16]=[CH:15][CH:14]=2)=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 18179872HCID 18179872, 화합물HCID 697405872-[4-(3-fluoro-phenyl)-2-oxo-1,2-dihydro-indol-(3Z) ylidenemethyl]-5-methyl-1H-pyrrole-3-carboxylic acid

생성물 1

HCID 60061360HCID 60061360, 화합물수율 71%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

A mixture of 2-[4-(3-fluoro-phenyl)-2-oxo-1,2-dihydro-indol-(3Z)-ylidenemethyl]-5-methyl-1H-pyrrole-3-carboxylic acid (53 mg, 0.15 mmol), HOBt (28 mg), EDC (36 mg), TEA (0.042 mL) and N1-(2,2,2-trifluoro-ethyl)-ethane-1,2-diamine (0.036 mL) in DMF (1 mL) was stirred at rt for 48 hours. The solvent was removed and diluted with sat. NaHCO3. It was then extracted with DCM, dried and concentrated. The residue was purified on a silica gel column to give 52 mg (71%) of the titled compound.

후처리

  1. customThe solvent was removed
  2. additiondiluted with sat. NaHCO3
  3. extractionIt was then extracted with DCM
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified on a silica gel column

출처 및 근거

ORD 기록
ord-62df405356be4cdb8a6d6c76b61b688c
출처 데이터셋
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06677368B2

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