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Triethylamine → tert-Butyl 4-(4-(3-cyclobutylureido)benzoyl)piperazine-1-carboxylate

HRID 1878413
ノート
印刷プレビュー

反応式

HRID 1878413 の反応式
[CH:1]1([NH:5][C:6](=[O:17])[NH:7][C:8]2[CH:16]=[CH:15][C:11]([C:12]([OH:14])=O)=[CH:10][CH:9]=2)[CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[N:25]1([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1.CCCP1(OP(CCC)(=O)OP(CCC)(=O)O1)=O>[Cl-].[Na+].O.O.ClCCl>[CH:1]1([NH:5][C:6](=[O:17])[NH:7][C:8]2[CH:9]=[CH:10][C:11]([C:12]([N:28]3[CH2:27][CH2:26][N:25]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:30][CH2:29]3)=[O:14])=[CH:15][CH:16]=2)[CH2:2][CH2:3][CH2:4]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 8471TriethylamineHCID 111923Propylphosphonic anhydrideHCID 143452tert-Butyl piperazine-1-carboxylateHCID 624152074-(3-Cyclobutylureido)benzoic acid

生成物 1

HCID 57917609tert-Butyl 4-(4-(3-cyclobutylureido)benzoyl)piperazine-1-carboxylate収率 94.9%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 6344Dichloromethane溶媒
HCID 57417360Sodium chloride; water溶媒

実験手順

A flask was charged with 4-(3-cyclobutylureido)benzoic acid (51.3 mmol, 12.023 g), triethyl-amine (129 mmol, 18 mL, 13.07 g) and dichloromethane (75 mL) and cooled to 0° C. tert-Butyl piperazine-1-carboxylate (51.3 mmol, 9.56 g) was then added and the reagents were stirred together for 10 minutes at 0° C. before 1-propanephosphonic acid cyclic anhydride (64.2 mmol, 38.0 mL, 40.8 g, 50% solution in ethyl acetate) was slowly added. The reaction mixture was allowed to warm slowly to room temperature. After 5 hours stirring, the reaction was poured into a flask containing water (100 mL) and brine (20 ml). The mixture was then stirred and left to stand overnight. The resulting precipitate was collected by vacuum filtration, washed with cold water and dried under vacuum to yield the title compound as a white powder (19.6 g). MS (ESI) m/z 403.5 [M+H]+

後処理

  1. additionwas then added
  2. additionwas slowly added
  3. additionthe reaction was poured into a flask
  4. stirringThe mixture was then stirred
  5. waitleft
  6. waitto stand overnight
  7. filtrationThe resulting precipitate was collected by vacuum filtration
  8. washwashed with cold water
  9. customdried under vacuum

出典と根拠

ORDレコード
ord-96a7b8f6adc84f91bc60b149c6a545da
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08314091B2

反応ノート

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