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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ammonium Chloride → HCID 21264607, 화합물

HRID 567118
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HRID 567118 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 25517Ammonium ChlorideHCID 21264588HCID 21264588, 화합물HCID 22280793N-diethoxymethyltriazoleHCID 178418339Butyllithium

생성물 1

HCID 21264607HCID 21264607, 화합물수율 34.1%

시약·촉매·용매 2

HCID 887Methanol용매
HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7fad4519a66742d98c210b31681b77c6
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06177459B1

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