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 → Aminocyclopyrachlor-methyl

HRID 907430
ノート
印刷プレビュー

反応式

HRID 907430 の反応式
C[O-].[Na+].[NH2:4][C:5]1[N:10]=[C:9]([CH:11]2[CH2:13][CH2:12]2)[N:8]=[C:7]([C:14]([O:16][CH2:17]C)=[O:15])[C:6]=1[Cl:19].Cl.[Cl-].[NH4+]>CO>[NH2:4][C:5]1[N:10]=[C:9]([CH:11]2[CH2:13][CH2:12]2)[N:8]=[C:7]([C:14]([O:16][CH3:17])=[O:15])[C:6]=1[Cl:19]
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 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 10942334Sodium MethoxideHCID 11989828Ethyl 6-amino-5-chloro-2-cyclopropylpyrimidine-4-carboxylate2 回

生成物 1

HCID 16725794Aminocyclopyrachlor-methyl収率 92%

試薬・触媒・溶媒 2

HCID 887
Methanol
触媒
HCID 887Methanol溶媒2 回

実験手順

Sodium methoxide in methanol (25%, 3 drops) was added to ethyl 6-amino-5-chloro-2-cyclopropyl-4-pyrimidinecarboxylate (i.e. the product of Example 7) (0.53 g) in methanol (15 mL). The mixture was boiled for 1 h. The mixture was allowed to cool to room temperature, and was partitioned between hydrochloric acid (0.28 g, 1.16 mmol) in methanol (5 mL). The mixture was boiled for 90 minutes. The mixture was allowed to cool to room temperature, and ammonium chloride (0.3 g, 5.6 mmol) was added. After 10 minutes the solvent was removed under reduced pressure. The mixture was extracted with ethyl acetate (50 mL), and the extracts evaporated to give the product as a white solid (0.24 g, 92% yield). Product recrystallized from ethyl acetate melted at 148.5-149.5° C.

後処理

  1. waitThe mixture was boiled for 90 minutes
  2. temperatureto cool to room temperature
  3. customAfter 10 minutes the solvent was removed under reduced pressure
  4. extractionThe mixture was extracted with ethyl acetate (50 mL)
  5. customthe extracts evaporated

出典と根拠

ORDレコード
ord-19bc1b4b31d0447b8a2d38718f7f72b6
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08013155B2

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