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

Potassium Carbonate → HCID 24964085、化合物

HRID 655277
ノート
印刷プレビュー

反応式

HRID 655277 の反応式
Cl.Cl.[C:3]1([C:9]2[N:14]=[N:13][C:12]([NH:15][NH2:16])=[CH:11][CH:10]=2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH3:17][C:18]1[CH:27]=[CH:26][C:25]2[C:20](=[CH:21][CH:22]=[C:23]([CH2:28][C:29](O)=O)[CH:24]=2)[N:19]=1.Cl.CN(C)CCCN=C=NCC.O.ON1C2C=CC=CC=2N=N1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:17][C:18]1[CH:27]=[CH:26][C:25]2[C:20](=[CH:21][CH:22]=[C:23]([CH2:28][C:29]3[N:13]4[N:14]=[C:9]([C:3]5[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=5)[CH:10]=[CH:11][C:12]4=[N:15][N:16]=3)[CH:24]=2)[N:19]=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 5

HCID 11430Potassium CarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 59320364HCID 59320364、化合物HCID 687055603-Hydrazino-6-phenylpyridazine dihydrochloride

生成物 1

HCID 24964085HCID 24964085、化合物
収率 32%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A vial was charged with (6-phenyl-pyridazin-3-yl)-hydrazine dihydrochloride (20 mg, 0.077 mmol), (2-methyl-quinolin-6-yl)-acetic acid (17 mg, 0.085 mmol), N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (22 mg, 0.115 mmol), 1-hydroxybenzotriazole hydrate (11 mg, 0.077 mmol), potassium carbonate (32 mg, 0.231 mmol), and N,N-dimethyl formamide (0.7 mL). The reaction mixture was stirred at room temperature for 14 h. After such time the mixture was concentrated in vacuo. Acetic acid (1 mL) was added to the residue and the resulting reaction mixture was stirred at 55° C. for 5 h. After such time the mixture was concentrated in vacuo and partitioned between 1 M aqueous potassium carbonate and ethyl acetate. The organic layer was washed with 1 M aqueous potassium carbonate, then brine, and directly adsorbed on silica gel. Purification on silica gel with 0-8% gradient of methanol in ethyl acetate afforded the title compound (8.7 mg, 0.024 mmol, 32% yield) as a light yellow solid. Analytical data presented in Table 1.

後処理

  1. concentrationAfter such time the mixture was concentrated in vacuo
  2. additionAcetic acid (1 mL) was added to the residue
  3. customthe resulting reaction mixture
  4. stirringwas stirred at 55° C. for 5 h
  5. concentrationAfter such time the mixture was concentrated in vacuo
  6. custompartitioned between 1 M aqueous potassium carbonate and ethyl acetate
  7. washThe organic layer was washed with 1 M aqueous potassium carbonate
  8. customPurification on silica gel with 0-8% gradient of methanol in ethyl acetate

出典と根拠

ORDレコード
ord-0c51c7547dd748938aea0bd0ba7eb37c
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08071581B2

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