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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ammonia → HCID 54202893, 화합물

HRID 1088461
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HRID 1088461 반응식
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][C:8]([CH:12]=[CH:13][C:14]3[CH:15]=[C:16]([CH:23]=[CH:24][CH:25]=3)[O:17][CH:18]([CH3:22])[C:19](O)=[O:20])=[N:9]2)=[CH:4][CH:3]=1.C([N:28](CC)CC)C.ClC(OCC)=O.N>C(Cl)Cl>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][C:8]([CH:12]=[CH:13][C:14]3[CH:15]=[C:16]([CH:23]=[CH:24][CH:25]=3)[O:17][CH:18]([CH3:22])[C:19]([NH2:28])=[O:20])=[N:9]2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 54478688HCID 54478688, 화합물

생성물 1

HCID 54202893HCID 54202893, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

(+)-2-(3-(2-(7-Chloroquinolin-2-yl)ethenyl)phenoxy)propanoic acid from Example 72 (2.372 g, 6.71 mmol) was dissolved in methylene chloride (40 mL) containing triethylamine (1.87 mL, 12.5 mmol), and ethyl chloroformate (710 μL, 7.38 mmol) in methylene chloride (20 mL) was added dropwise at -15° C. with stirring. The mixture was stirred for a further 20 minutes at -15° C., and then it was poured into methylene chloride (125 mL) that had been saturated with ammonia at 0° C. The reaction mixture was stirred for a few minutes, and then poured into ice-water The mixture was filtered, and the filtrate was separated. Evaporation of the methylene chloride layer gave more solid, and the two fractions were combined and recrystallized from acetonitrile to give the title product, mp 195°-197° C., [α]D -9.8° (c 0.515 in dimethylformamide).

후처리

  1. additionwas added dropwise at -15° C.
  2. stirringThe mixture was stirred for a further 20 minutes at -15° C.
  3. stirringThe reaction mixture was stirred for a few minutes
  4. filtrationwas filtered
  5. customthe filtrate was separated
  6. customEvaporation of the methylene chloride layer
  7. customgave more solid
  8. customrecrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-98c5ec1a52434ea39ad60ed46a0601c9
출처 데이터셋
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04962203

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