ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Hydrochloric Acid → HCID 135867273、化合物

HRID 2076826
ノート
印刷プレビュー

反応式

HRID 2076826 の反応式
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][O:11][CH2:12][C:13]([NH2:15])=[NH:14])[CH:6]=[CH:7][CH:8]=1.C[O-].[Na+].C([O:21][C:22]([C:24]1[CH:29]=[CH:28][N:27]=[N:26][C:25]=1Cl)=O)C.C([O-])([O-])=O.[K+].[K+].Cl>CO.CN(C=O)C.O>[Cl:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][O:11][CH2:12][C:13]2[NH:15][C:22](=[O:21])[C:24]3[CH:29]=[CH:28][N:27]=[N:26][C:25]=3[N:14]=2)[CH:6]=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 10942334Sodium MethoxideHCID 14542887Ethyl 3-chloropyridazine-4-carboxylateHCID 67098848HCID 67098848、化合物

生成物 1

HCID 135867273HCID 135867273、化合物収率 3.6%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒

実験手順

2-[2-(3-Chloro-phenyl)-ethoxy]-acetamidine hydrochloride (240 mg, 0.964 mmol; described in example 6.2) was dissolved in MeOH (2 ml) and NaOMe (30% solution in MeOH, 179 μl, 0.964 mmol) was added dropwise at 0° C. The suspension was stirred at ambient temperature for 15 min and then evaporated. To the remaining residue were added a solution of crude 3-chloro-pyridazine-4-carboxylic acid ethyl ester (180 mg) in DMF (3 ml) and subsequently K2CO3 (267 mg, 1.929 mmol) and the mixture was heated to 100° C. for 18 h. Then water was added, the pH was adjusted to 3 by addition of 0.1 N HCl and the mixture was extracted three times with CH2Cl2 and one time with ethyl acetate. The combined organic extracts were washed three times with diluted HCl (pH 3), dried (Na2SO4) and evaporated. The remaining residue was triturated with Et2O and the brown solid was filtered off and further purified by column chromatography (silica gel, CH2Cl2/MeOH 95:5) to give the title compound (11 mg, 0.035 mmol; 3.6%) as brown solid. MS: m/e=317.1 [M+H+].

後処理

  1. customevaporated
  2. temperaturethe mixture was heated to 100° C. for 18 h
  3. extractionthe mixture was extracted three times with CH2Cl2 and one time with ethyl acetate
  4. washThe combined organic extracts were washed three times with diluted HCl (pH 3)
  5. dry with materialdried (Na2SO4)
  6. customevaporated
  7. customThe remaining residue was triturated with Et2O
  8. filtrationthe brown solid was filtered off
  9. customfurther purified by column chromatography (silica gel, CH2Cl2/MeOH 95:5)

出典と根拠

ORDレコード
ord-2e2077d645d74e34899ec02bced00409
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07928106B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート