Carbon Dioxide → HCID 15022347, 화합물

HRID 1770321노트

반응식

HRID 1770321 반응식
[Cl:1][C:2]1[C:3]([C:7]([NH:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[O:8])=[CH:4][S:5][CH:6]=1.C([Li])CCC.[C:21](=[O:23])=[O:22]>O1CCCC1>[Cl:1][C:2]1[C:3]([C:7]([NH:9][C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)=[O:8])=[C:4]([C:21]([OH:23])=[O:22])[S:5][CH:6]=1

참가 물질

5

반응물 3

HCID 280Carbon DioxideHCID 15022346HCID 15022346, 화합물HCID 178418339Butyllithium

생성물 1

HCID 15022347HCID 15022347, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
-70 °C

실험 절차

4-Chlorothiophene-3-carboxanilide (14.6 g, 0.061 mol) is dissolved in 450 ml of tetrahydrofuran, the solution is cooled to -70° C. and n-butyllithium (0.13 mol, 1.6N solution in n-hexane) is added. After 30 minutes, carbon dioxide gas is passed in until the solution is saturated, and the solution is allowed to warm up slowly to room temperature. It is worked up by evaporating to dryness, taking up the solution residue n a mixture of water, sodium hydroxide solution and ethyl acetate, separating the phases and acidifying the aqueous phase with hydrochloric acid. The carboxylic acid is precipitated. Yield: 13.6 g, 78%, mp. 208° to 210° C.

후처리

  1. temperatureto warm up slowly to room temperature
  2. customby evaporating to dryness
  3. additiona mixture of water, sodium hydroxide solution and ethyl acetate
  4. customseparating the phases
  5. customThe carboxylic acid is precipitated

출처 및 근거

ORD 기록
ord-5b571bf9dfc741bd9a85e328947bcf45
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05386036

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