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Methanol → HCID 86604273、化合物

HRID 2054172
ノート
印刷プレビュー

反応式

HRID 2054172 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([S:9][C:10]2[CH:15]=[CH:14][C:13]([CH2:16][N:17]3[CH2:22][CH2:21][CH:20]([C:23]4[CH:24]=[C:25]([NH2:30])[CH:26]=[CH:27][C:28]=4[CH3:29])[CH2:19][CH2:18]3)=[CH:12][CH:11]=2)=[CH:5][CH:4]=1.[C:31]([O:35][N:36]([CH2:40][C:41](O)=[O:42])[C:37]([CH3:39])=[O:38])([CH3:34])([CH3:33])[CH3:32].Cl.CN(C)CCCN=C=NCC.CO>C(Cl)Cl.CN(C)C=O.CN(C)C1C=CN=CC=1.C(Cl)Cl>[C:31]([O:35][N:36]([CH2:40][C:41]([NH:30][C:25]1[CH:26]=[CH:27][C:28]([CH3:29])=[C:23]([CH:20]2[CH2:21][CH2:22][N:17]([CH2:16][C:13]3[CH:12]=[CH:11][C:10]([S:9][C:6]4[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=4)=[CH:15][CH:14]=3)[CH2:18][CH2:19]2)[CH:24]=1)=[O:42])[C:37]([CH3:39])=[O:38])([CH3:34])([CH3:33])[CH3:32]
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 887MethanolHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 22142721HCID 22142721、化合物HCID 24990093HCID 24990093、化合物

生成物 1

HCID 86604273HCID 86604273、化合物収率 50.1%

試薬・触媒・溶媒 3

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 6344Dichloromethane溶媒2 回
HCID 22350042dichloromethane N,N-dimethylformamide溶媒

実験手順

To a stirred solution of 3-(1-{[4-(4-methoxyphenylthio)phenyl]methyl}(4-piperidyl))-4-methylphenylamine (121 mg, 0.289 mmol) in CH2Cl2/dimethylformamide (2.00/0.200 mL) was added 2-[(tert-butoxy)-N-methylcarbonylamino]acetic acid (54.6 mg, 0.289 mmol) and 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (111 mg, 0.578 mmol) and 4-dimethylaminopyridine (5.00 mg). The reaction mixture was stirred at room temperature for 10 h, then partitioned between CH2Cl2 (10 mL) and saturated NaHCO3 solution (10 mL) and the organic phase was separated and washed with water (10 mL), then brine (10 mL), dried over MgSO4 and concentrated in vacuo to give the crude product. Purification by flash column chromatography (eluent: CH2Cl2 then 3% methanol in CH2Cl2) gave 2-[(tert-butoxy)-N-methylcarbonylamino]-N-[3-(1-{[4-(4-methoxyphenylthio)phenyl]methyl}(4-piperidyl))-4-methylphenyl]acetamide (84.7 mg, 50.1% yield) as a yellow solid.

後処理

  1. custompartitioned between CH2Cl2 (10 mL) and saturated NaHCO3 solution (10 mL)
  2. customthe organic phase was separated
  3. washwashed with water (10 mL)
  4. dry with materialbrine (10 mL), dried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customto give the crude product
  7. customPurification by flash column chromatography (eluent

出典と根拠

ORDレコード
ord-e26b732defb34f198ed01b6a603cb546
出典データセット
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07329656B2

反応ノート

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