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Ammonia → HCID 54202893、化合物

HRID 1088461
ノート
印刷プレビュー

反応式

HRID 1088461 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 222AmmoniaHCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 54478688HCID 54478688、化合物

生成物 1

HCID 54202893HCID 54202893、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

(+)-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).

後処理

  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

出典と根拠

ORDレコード
ord-98c5ec1a52434ea39ad60ed46a0601c9
出典データセット
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04962203

反応ノート

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