Tetrahydrofuran → HCID 69311621, 화합물

HRID 2250590노트

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HRID 2250590 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:10]3[N:11]([C:26]([CH2:29][CH3:30])=[CH:27][CH:28]=3)[N:12]=[C:13]([CH2:20][C:21]([O:23]CC)=[O:22])[C:14]=2[C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:5][CH:4]=1)#[N:2].O1CCCC1.[OH-].[K+]>C(O)C>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([C:9]2[C:10]3[N:11]([C:26]([CH2:29][CH3:30])=[CH:27][CH:28]=3)[N:12]=[C:13]([CH2:20][C:21]([OH:23])=[O:22])[C:14]=2[C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:7][CH:8]=1)#[N:2]

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 14797Potassium Hydroxide2회HCID 69308255HCID 69308255, 화합물

생성물 1

HCID 69311621HCID 69311621, 화합물수율 93.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of ethyl 4-(4-cyanophenyl)-2-(2-ethoxy-2-oxoethyl)-7-ethylpyrrolo[1,2-b]pyridazine-3-carboxylate (77.9 mg) in ethanol (0.5 mL)-tetrahydrofuran (0.5 mL) was added 1N potassium hydroxide. The resulting solution was stirred for 2.5 hours at room temperature. The mixture was stirred for further 1 hour after adding 1N potassium hydroxide (0.04 mL). The reaction was quenched by adding 1N hydrochloric acid (0.23 mL). The volatile was evaporated off, and the resulting residue was partitioned between ethyl acetate (10 mL) and 1N hydrochloric acid (6 mL). The organic layer was washed with brine, dried, and evaporated to give [4-(4-cyanophenyl)-3-(ethoxycarbonyl)-7-ethylpyrrolo[1,2-b]pyridazin-2-yl]acetic acid as an yellow solid (67.7 mg, 93.4%).

후처리

  1. stirringThe mixture was stirred for further 1 hour
  2. customThe reaction was quenched
  3. additionby adding 1N hydrochloric acid (0.23 mL)
  4. customThe volatile was evaporated off
  5. customthe resulting residue was partitioned between ethyl acetate (10 mL) and 1N hydrochloric acid (6 mL)
  6. washThe organic layer was washed with brine
  7. customdried
  8. customevaporated

출처 및 근거

ORD 기록
ord-9ccaa8aba8214eb7acb2188e5259b5c7
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07317009B2

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