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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
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Hydrochloric Acid → HCID 13066646、化合物

HRID 1606637
ノート
印刷プレビュー

反応式

HRID 1606637 の反応式
[NH2:1][C:2]1[CH:11]=[C:10]([NH2:12])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].C(N([CH2:18][CH3:19])CC)C.[C:20]([O:23][C:24]1[CH:32]=[CH:31][CH:30]=[CH:29][C:25]=1[C:26](Cl)=[O:27])(=[O:22])[CH3:21].Cl>O1CCCC1>[C:20]([O:23][C:19]1[CH:18]=[CH:31][CH:32]=[CH:24][C:25]=1[C:26]([NH:1][C:2]1[CH:11]=[C:10]([NH:12][C:26](=[O:27])[C:25]2[CH:29]=[CH:30][CH:31]=[CH:32][C:24]=2[O:23][C:20](=[O:22])[CH3:21])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5])=[O:27])(=[O:22])[CH3:21]
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 313Hydrochloric AcidHCID 8471TriethylamineHCID 796682-Acetoxybenzoyl chlorideHCID 12399493Methyl 2,4-diaminobenzoate

生成物 1

HCID 13066646HCID 13066646、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A mixture of 6.64 g of methyl 2,4-diaminobenzoate, 11.5 ml of triethylamine and 50 ml of tetrahydrofuran was added dropwise to a solution of 17.4 g of 2-acetoxybenzoylchloride in 300 ml of tetrahydrofuran over 0.5 - 1 hour, while stirring at 5° - 10°C. The stirring was then continued at room temperature for 2 hours. The resulting reaction mixture was poured into 1.5 l of diluted hydrochloric acid to precipitate crystals. The crystals were recovered by filtration, washed with water, dried and recrystallized from ethyl acetate to yield 15 g of methyl 2,4-bis(2'-acetoxybenzamido)-benzoate having a melting point between 143° - 145°C.

後処理

  1. customThe resulting reaction mixture
  2. customto precipitate crystals
  3. filtrationThe crystals were recovered by filtration
  4. washwashed with water
  5. customdried
  6. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-41a7f1aefa4e4355a40e174210165ba3
出典データセット
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03953496

反応ノート

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