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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ammonium → HCID 178420706, 화합물

HRID 2351875
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HRID 2351875 반응식
[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH2:11][O:12][C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][CH:20]=1)[C:16]#[N:17].[N-:21]=[N+:22]=[N-:23].[Na+].[Cl-].[NH4+].[NH4+].Cl>CN(C)C=O.CO>[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH2:11][O:12][C:13]1[CH:14]=[C:15]([C:16]2[NH:23][N:22]=[N:21][N:17]=2)[CH:18]=[CH:19][CH:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 223AmmoniumHCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium Azide2회HCID 14501705HCID 14501705, 화합물

생성물 1

HCID 178420706HCID 178420706, 화합물수율 48.8%

시약·촉매·용매 2

HCID 887
Methanol
용매
HCID 6228Dimethylformamide용매

반응 조건

온도
140 °C

실험 절차

A mixture of 8.8 g of 3-(2-quinolylmethyloxy)benzonitrile, 2.3 g of sodium azide and 1.9 g of ammonium chloride in 100 ml of dimethylformamide is stirred at 140° C. for 7 hours. An additional amount of sodium azide (1.2 g) and ammonium (1.0 g) is added and stirring resumed at 140° C. for 17 hours. The mixture is poured over ice and acidified with hydrochloric acid. The crude product solidifies and is filtered off to give 11 g of crude product. The crude product is slurried with hot methanol and filtered off. To a hot solution of this material is added enough water to cause trubidity. On cooling the compound crystallizes and is filtered off to yield 5.0 g of pure material having a M.P. of 200°-205° C. dec.

후처리

  1. stirringstirring
  2. waitresumed at 140° C. for 17 hours
  3. additionThe mixture is poured over ice
  4. filtrationis filtered off
  5. customto give 11 g of crude product
  6. filtrationfiltered off
  7. additionTo a hot solution of this material is added enough water
  8. temperatureOn cooling the compound
  9. customcrystallizes
  10. filtrationis filtered off

출처 및 근거

ORD 기록
ord-d6ad8b0b8c4b475ea5a0bdce010372e7
출처 데이터셋
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04874769

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