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Acetic Acid → HCID 68530554、化合物

HRID 2180190
ノート
印刷プレビュー

反応式

HRID 2180190 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10](=[O:27])[N:11]([CH2:13][C:14]2([C:20]3[CH:25]=[CH:24][C:23]([I:26])=[CH:22][CH:21]=3)[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)[CH3:12])[CH:5]=[C:6]([Cl:8])[CH:7]=1.[CH:28]1([CH:31]=O)[CH2:30][CH2:29]1.CC(O)=O.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+]>C(Cl)CCl.CCOC(C)=O>[CH:28]1([CH2:31][N:17]2[CH2:18][CH2:19][C:14]([CH2:13][N:11]([CH3:12])[C:10]([NH:9][C:4]3[CH:5]=[C:6]([Cl:8])[CH:7]=[C:2]([Cl:1])[CH:3]=3)=[O:27])([C:20]3[CH:21]=[CH:22][C:23]([I:26])=[CH:24][CH:25]=3)[CH2:15][CH2:16]2)[CH2:30][CH2:29]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 176Acetic AcidHCID 123114CyclopropanecarboxaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 224903673-(3,5-Dichloro-phenyl)-1-[4-(4-iodo-phenyl)-piperidin-4-ylmethyl]-1-methyl-urea

生成物 1

HCID 68530554HCID 68530554、化合物収率 96.6%

試薬・触媒・溶媒 2

HCID 11
1,2-Dichloroethane
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 3-(3,5-dichloro-phenyl)-1-[4-(4-iodo-phenyl)-piperidin-4-ylmethyl]-1-methyl-urea (˜0.10 g, 0.17 mmol) in ClCH2CH2Cl (1 mL) was added cyclopropanecarboxaldehyde (0.016 mL, 0.204 mmol, 1.2 eq.). The mixture was stirred at room temperature for 15 min and then HOAc (0.01 mL, 1% v/v) was added. The reaction was stirred for a further 1 h. Na(OAc)3BH (0.054 g, 0.255 mmol, 1.5 eq.) was added and the reaction was stirred at room temperature for 12 h. It was diluted with EtOAc (10 mL) and washed with saturated NaHCO3 (10 mL) and saturated brine (10 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated by rotary evaporation to give 1-[1-cyclopropylmethyl-4-(4-iodo-phenyl)-piperidin-4-ylmethyl]-3-(3,5-dichloro-phenyl)-1-methyl-urea (0.094 g, 95%). Crude 1H NMR (CDCl3): δ 7.83 (d, 2H), 7.22 (m, 4H), 7.05 (s, 1H), 6.01 (br.s, 1H), 3.50 (s, 2H), 2.97 (d, 2H), 2.83 (s, 3H), 2.36 (m, 2H), 2.27 (m, 2H), 2.09 (m, 2H), 0.91 (br.m, 1H), 0.58 (d, 2H), 0.15 (d, 2H).

後処理

  1. stirringThe reaction was stirred for a further 1 h
  2. stirringthe reaction was stirred at room temperature for 12 h
  3. washwashed with saturated NaHCO3 (10 mL) and saturated brine (10 mL)
  4. dry with materialThe combined organic extracts were dried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated by rotary evaporation

出典と根拠

ORDレコード
ord-01db5e57f6f04d28a2d7cf3780e005f7
出典データセット
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06887889B2

反応ノート

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