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Ethanethiol → HCID 15239984、化合物

HRID 1653640
ノート
印刷プレビュー

反応式

HRID 1653640 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=O)[C:5]([O:11][C:12]2[N:17]=[C:16]([O:18][CH3:19])[CH:15]=[C:14]([O:20][CH3:21])[N:13]=2)=[CH:4][CH:3]=1.[CH2:22]([SH:24])[CH3:23].P(OC#N)(OCC)(OCC)=O.C(N(CC)CC)C>O.C1COCC1>[NH2:1][C:2]1[N:7]=[C:6]([C:8](=[O:10])[S:24][CH2:22][CH3:23])[C:5]([O:11][C:12]2[N:17]=[C:16]([O:18][CH3:19])[CH:15]=[C:14]([O:20][CH3:21])[N:13]=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

7

反応物 4

HCID 6343EthanethiolHCID 8471TriethylamineHCID 15239982HCID 15239982、化合物HCID 18315342HCID 18315342、化合物

生成物 1

HCID 15239984HCID 15239984、化合物収率 34.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

2.5 g (8.5 mmol) of 6-amino-3-[(4,6-dimethoxypyrimidin-2-yl)oxy]picolinic acid, 0.64 g (10.3 mmol) of ethylmercaptan, 2.8 g (17 mmol) of diethyl cyano phosphate and 1.73 g (17.1 mmol) of triethylamine were added to a THF solution, and the mixture was stirred at room temperature for 4 hours. After completion of the reaction, the reaction mixture was poured into water and extracted with ethyl acetate, followed by separation, washed with water and dried. Then, the solvent was distilled off, and the residual oily product was purified by column chromatography to obtain the desired product as colorless transparent crystals.

後処理

  1. customAfter completion of the reaction
  2. extractionextracted with ethyl acetate
  3. customfollowed by separation
  4. washwashed with water
  5. customdried
  6. distillationThen, the solvent was distilled off
  7. customthe residual oily product was purified by column chromatography

出典と根拠

ORDレコード
ord-14d9beffe3244596afb800943c123805
出典データセット
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05403816

反応ノート

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