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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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Ammonium Chloride → HCID 21264607、化合物

HRID 567118
ノート
印刷プレビュー

反応式

HRID 567118 の反応式
C([Li])CCC.C(O[CH:9]([O:15]CC)[N:10]1[CH:14]=[CH:13][N:12]=[N:11]1)C.[CH3:18][C:19]1[CH:39]=[CH:38][CH:37]=[CH:36][C:20]=1[O:21][CH2:22][C:23]1[CH:35]=[CH:34][CH:33]=[CH:32][C:24]=1C(N1CCCC1)=O.[Cl-].[NH4+]>O1CCCC1.CO>[CH3:18][C:19]1[CH:39]=[CH:38][CH:37]=[CH:36][C:20]=1[O:21][CH2:22][C:23]1[CH:35]=[CH:34][CH:33]=[CH:32][C:24]=1[C:9]([N:10]1[CH:14]=[CH:13][N:12]=[N:11]1)=[O:15]
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 25517Ammonium ChlorideHCID 21264588HCID 21264588、化合物HCID 22280793N-diethoxymethyltriazoleHCID 178418339Butyllithium

生成物 1

HCID 21264607HCID 21264607、化合物収率 34.1%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

At −20° C., 2.8 g (0.01 mol) of 23% pure n-butyllithium are added dropwise within 15 minutes to a solution of 1.7 g (0.01 mol) of N-diethoxymethyltriazole in 10 ml of tetrahydrofuran. Stirring is continued for 15 minutes at −20° C., and 1.48 g (0.005 mol) of N-[2-(2-methylphenoxymethyl)-benzoyl]-pyrrolidine dissolved in 10 ml of tetrahydrofuran are then added, and the mixture is stirred for a further 30 minutes at −20° C. 2 g of ammonium chloride and 10 ml of methanol are added and the mixture is heated under reflux for 15 minutes. The volatile components are removed under reduced pressure, the residue is admixed with water and extracted with ethyl acetate, and the organic phase is dried over sodium sulphate and concentrated under reduced pressure. The residue crystallizes when treated with a mixture of diethyl ether and petroleum ether in the ratio of 1:1. 0.5 g (17% of theory) of 3-[2-(2-methylphenoxymethyl)-benzoyl]-triazole of melting point 179° C. is obtained.

後処理

  1. additionare then added
  2. stirringthe mixture is stirred for a further 30 minutes at −20° C
  3. temperaturethe mixture is heated
  4. temperatureunder reflux for 15 minutes
  5. customThe volatile components are removed under reduced pressure
  6. extractionextracted with ethyl acetate
  7. dry with materialthe organic phase is dried over sodium sulphate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue crystallizes when
  10. additiontreated with a mixture of diethyl ether and petroleum ether in the ratio of 1:1

出典と根拠

ORDレコード
ord-7fad4519a66742d98c210b31681b77c6
出典データセット
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06177459B1

反応ノート

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