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1,2-Dichloroethane → HCID 178495642, 화합물

HRID 1258753
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HRID 1258753 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([N:9]2[CH2:13][CH2:12][CH2:11][C@H:10]2[CH2:14][O:15][CH3:16])=[CH:4][C:3]=1[NH:17][C:18](=S)[NH:19][C:20]1[CH:21]=[C:22]([CH:34]=[CH:35][C:36]=1[Cl:37])[CH2:23][NH:24][C:25]([C:27]1([C:30]([F:33])([F:32])[F:31])[CH2:29][CH2:28]1)=[O:26].C(Cl)CCl.CN(C=O)C>[Cl-].[Na+].O>[Cl:37][C:36]1[CH:35]=[CH:34][C:22]([CH2:23][NH:24][C:25]([C:27]2([C:30]([F:33])([F:32])[F:31])[CH2:29][CH2:28]2)=[O:26])=[CH:21][C:20]=1[NH:19][C:18]1[NH:17][C:3]2[CH:4]=[C:5]([N:9]3[CH2:13][CH2:12][CH2:11][C@H:10]3[CH2:14][O:15][CH3:16])[C:6]([Cl:8])=[CH:7][C:2]=2[N:1]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 111,2-DichloroethaneHCID 6228DimethylformamideHCID 86674358(S)-N-(3-(3-(2-Amino-4-chloro-5-(2-(methoxymethyl)pyrrolidin-1-yl)phenyl)thioureido)-4-chlorobenzyl)-1-(trifluoromethyl)cyclopropanecarboxamide

생성물 1

HCID 178495642HCID 178495642, 화합물

시약·촉매·용매 1

HCID 57417360Sodium chloride; water용매

반응 조건

온도
90 °C

실험 절차

A mixture of (S)—N-(3-(3-(2-amino-4-chloro-5-(2-(methoxymethyl)pyrrolidin-1-yl)phenyl)thioureido)-4-chlorobenzyl)-1-(trifluoromethyl)cyclopropanecarboxamide (110 mg; 0.19 mmol), EDC (36 mg; 0.19 mmol) and DMF (4 mL) was stirred at 90° C. overnight. The mixture was poured into brine and extracted with CH2Cl2. The organic layer was dried over Na2SO4, filtered and concentrated and the residue was purified by column chromatography.

후처리

  1. extractionextracted with CH2Cl2
  2. dry with materialThe organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customthe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-22de824c786a4525be28856cb845512c
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08466186B2

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