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

HRID 458143ノート

反応式

HRID 458143 の反応式
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

参加物

6

反応物 2

HCID 3939Lithium HydroxideHCID 18401639HCID 18401639、化合物

生成物 1

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

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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+.

後処理

  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

出典と根拠

ORDレコード
ord-d82fdf1bee7d4126860f1c4ed2b664a9
出典データセット
uspto-grants-2007_03
特許番号
US07189850B2

反応ノート

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