Carbon Dioxide → HCID 15022347, 화합물

HRID 1197421노트

반응식

HRID 1197421 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

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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 solid residue in 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: 13.5 g, 78%; mp. 208° to 210° C.

후처리

  1. temperatureto warm up slowly to room temperature
  2. customby evaporating to dryness
  3. additionin a 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-916390a0cff248938766d6b8129c5294
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05276009

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