Lithium Hydroxide → 1-(4-Chlorophenyl)-1,3,8-triazaspiro[4.5]decan-4-one

HRID 458143노트

반응식

HRID 458143 반응식
FC(F)(F)C1C=C(C=C(C(F)(F)F)C=1)C([N:8]1[CH2:25][CH2:24][C:11]2([N:15]([C:16]3[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=3)[CH2:14][NH:13][C:12]2=[O:23])[CH2:10][CH2:9]1)=O.[Li+].[OH-]>C1COCC1.O.CO>[Cl:22][C:19]1[CH:20]=[CH:21][C:16]([N:15]2[C:11]3([CH2:10][CH2:9][NH:8][CH2:25][CH2:24]3)[C:12](=[O:23])[NH:13][CH2:14]2)=[CH:17][CH:18]=1

참가 물질

6

반응물 2

HCID 3939Lithium HydroxideHCID 18401639HCID 18401639, 화합물

생성물 1

HCID 201607621-(4-Chlorophenyl)-1,3,8-triazaspiro[4.5]decan-4-one수율 69.7%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of 1.5 g (2.97 mmol) 8-(3,5-bis-trifluoromethyl-benzoyl)-1-(4-chloro-phenyl)-1,3,8-triaza-spiro[4.5]decan-4-one in 4.5 ml THF, 4.5 ml water and 4.5 ml methanol were added 0.85 g (35.6 mmol) powdered LiOH. The reaction mixture was stirred at ambient temperature for 48 hours. The solvent was removed in vacuo. The residue was stirred in water. The resulting solid was filtered, washed with water and dried to provide the title compound (0.55 g) as a colorless solid; MS (ISP): 266.1 MH+.

후처리

  1. additionwere added 0.85 g (35.6 mmol)
  2. customThe solvent was removed in vacuo
  3. stirringThe residue was stirred in water
  4. filtrationThe resulting solid was filtered
  5. washwashed with water
  6. customdried

출처 및 근거

ORD 기록
ord-d82fdf1bee7d4126860f1c4ed2b664a9
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07189850B2

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