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1-Hydroxybenzotriazole → 2-Amino-4-[1-(3,4-dihydroxybenzoyl)-4-piperidinyl]-6-(4-methoxyphenylmethyl)pyrimidine

HRID 617187
ノート
印刷プレビュー

反応式

HRID 617187 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([CH2:8][C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)[CH:5]=[C:4]([CH:17]2[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]2)[N:3]=1.C([O:30][C:31]1[CH:32]=[C:33]([CH:37]=[CH:38][C:39]=1[O:40]CC1C=CC=CC=1)[C:34](O)=[O:35])C1C=CC=CC=1.ON1C2C=CC=CC=2N=N1>ClCCl>[NH2:1][C:2]1[N:3]=[C:4]([CH:17]2[CH2:22][CH2:21][N:20]([C:34](=[O:35])[C:33]3[CH:37]=[CH:38][C:39]([OH:40])=[C:31]([OH:30])[CH:32]=3)[CH2:19][CH2:18]2)[CH:5]=[C:6]([CH2:8][C:9]2[CH:10]=[CH:11][C:12]([O:15][CH3:16])=[CH:13][CH:14]=2)[N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 757711-HydroxybenzotriazoleHCID 108541553,4-Bis(benzyloxy)benzoic acidHCID 218515322-Amino-4-(4-methoxyphenylmethyl)-6-(4-piperidinyl)pyrimidine

生成物 1

HCID 218515152-Amino-4-[1-(3,4-dihydroxybenzoyl)-4-piperidinyl]-6-(4-methoxyphenylmethyl)pyrimidine収率 203.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

実験手順

To a solution of 2-amino-4-(4-methoxyphenylmethyl)-6-(4-piperidinyl)pyrimidine (160 mg, 0.54 mmol), 3,4-dibenzyloxybenzoic acid (179 mg, 0.54 mmol) and 1-hydroxybenzotriazole (72 mg, 0.54 mmol) in dichioromethane (150 ml) were added 1-ethyl-3-(N, N'-dimethylaminopropyl)carbodiimide hydrochloride (103 mg, 0.54 mmol) at room temperature under nitrogen atmosphere. After stirring for about 30 minutes, the mixture was washed successively with saturated sodium hydrogen carbonate solution and brine. The organic layer was dried over anhydrous sodium sulfate and then evaporated. The residue was purified by column chromatography (chloroform:methanol=99:1) to give the titled compound (477 mg).

後処理

  1. washthe mixture was washed successively with saturated sodium hydrogen carbonate solution and brine
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. customevaporated
  4. customThe residue was purified by column chromatography (chloroform:methanol=99:1)

出典と根拠

ORDレコード
ord-e62d668a608c4f56a3b66dc3b0649675
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05948786

反応ノート

読み込み中…

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