1-Butanol → HCID 90229418、化合物

HRID 1505752ノート

反応式

HRID 1505752 の反応式
[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]

参加物

8

反応物 4

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

生成物 1

HCID 90229418HCID 90229418、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bd5de2f9bd484c2dbcf3605a28c93fba
出典データセット
uspto-grants-2015_12
特許番号
US09216968B2

反応ノート

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