1-Butanol → HCID 90229418, 화합물

HRID 1505752노트

반응식

HRID 1505752 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:8](F)=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[CH2:12]([OH:16])[CH2:13][CH2:14][CH3:15].CC(C)([O-])C.[K+].Cl>C1COCC1.CN(C=O)C.O>[CH2:12]([O:16][C:8]1[CH:9]=[CH:10][C:2]([Cl:1])=[C:3]([CH:7]=1)[C:4]([OH:6])=[O:5])[CH2:13][CH2:14][CH3:15]

참가 물질

8

반응물 4

HCID 2631-ButanolHCID 313Hydrochloric AcidHCID 3028882-Chloro-5-fluorobenzoic acidHCID 23665647Potassium tert-butoxide

생성물 1

HCID 90229418HCID 90229418, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 2-chloro-5-fluorobenzoic acid (50 mg) and 1-butanol (263 μL) in THF (0.5 mL) and DMF (3 mL) was added potassium t-butoxide (329 mg) and the solution was reacted at 120° C. for 10 minutes in a microwave synthesizer (Biotage, Initiator). The reaction mixture was cooled and acidified by addition of water and 2M hydrochloric acid, extracted with diethyl ether, and dried over anhydrous sodium sulfate. The solvent was removed in vacuo, and the residue was purified on column chromatography to obtain the titled compound (17 mg) as white powder.

후처리

  1. customthe solution was reacted at 120° C. for 10 minutes in a microwave synthesizer (Biotage, Initiator)
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with diethyl ether
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed in vacuo
  6. customthe residue was purified on column chromatography

출처 및 근거

ORD 기록
ord-bd5de2f9bd484c2dbcf3605a28c93fba
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09216968B2

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