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Trifluoroacetic anhydride → HCID 23050245, 화합물

HRID 1651629
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HRID 1651629 반응식
[CH3:1][O:2][C:3]1[C:14]([O:15][CH3:16])=[CH:13][C:6]2[S:7][C:8]([C:10]([NH2:12])=O)=[CH:9][C:5]=2[CH:4]=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O>N1C=CC=CC=1.O>[CH3:1][O:2][C:3]1[C:14]([O:15][CH3:16])=[CH:13][C:6]2[S:7][C:8]([C:10]#[N:12])=[CH:9][C:5]=2[CH:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 9845Trifluoroacetic anhydrideHCID 23050251HCID 23050251, 화합물

생성물 1

HCID 23050245HCID 23050245, 화합물수율 78.2%

시약·촉매·용매 2

HCID 962Water용매2회HCID 1049Pyridine용매

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온도
0 °C

실험 절차

5,6-Dimethoxy-benzo[b]thiophene-2-carboxamide (65 g) was suspended in pyridine (325 ml). The solution was cooled to 0° C. and treated dropwise with trifluoro acetic anhydride (185 ml) whilst maintaining the internal reaction temperature below 10° C. The mixture was then stirred at room temperature for 30 min. then cooled and treated dropwise with water (170 ml) whilst maintaining the internal temperature below 30° C. The reaction mixture was diluted with more water (800 ml), stirred and the brown solid was filtered and dried under vacuum over calcium chloride at 60° C. Recrystallisation from acetone/ether afforded 5,6-dimethoxy-benzo[b]thiophene-2-carbonitrile as a white solid (47 g), m.p. 125° C.

후처리

  1. temperaturewhilst maintaining the internal reaction temperature below 10° C
  2. temperaturethen cooled
  3. temperaturewhilst maintaining the internal temperature below 30° C
  4. stirringstirred
  5. filtrationthe brown solid was filtered
  6. dry with materialdried under vacuum over calcium chloride at 60° C
  7. customRecrystallisation from acetone/ether

출처 및 근거

ORD 기록
ord-66a70c66869b49689b79b33bb23704f5
출처 데이터셋
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04929636

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