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Triethylamine → Ethyl 2-(4-(3-(2-(tert-butoxycarbonylamino)cyclohexyl)ureido)-2-chlorophenyl)acetate

HRID 1023859
ノート
印刷プレビュー

反応式

HRID 1023859 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:4]([Cl:14])[CH:3]=1.C(N(CC)CC)C.Cl[C:23](Cl)([O:25]C(=O)OC(Cl)(Cl)Cl)Cl.[NH2:34][CH:35]1[CH2:40][CH2:39][CH2:38][CH2:37][CH:36]1[NH:41][C:42](=[O:48])[O:43][C:44]([CH3:47])([CH3:46])[CH3:45]>ClCCl>[C:44]([O:43][C:42]([NH:41][CH:36]1[CH2:37][CH2:38][CH2:39][CH2:40][CH:35]1[NH:34][C:23](=[O:25])[NH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:4]([Cl:14])[CH:3]=1)=[O:48])([CH3:45])([CH3:47])[CH3:46]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 94429TriphosgeneHCID 3268011tert-Butyl (2-aminocyclohexyl)carbamateHCID 59419389Ethyl 2-(4-amino-2-chlorophenyl)acetate

生成物 1

HCID 67204990Ethyl 2-(4-(3-(2-(tert-butoxycarbonylamino)cyclohexyl)ureido)-2-chlorophenyl)acetate

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
3 回

実験手順

To a solution of ethyl 2-(4-amino-2-chlorophenyl)acetate (178 mg, 0.833 mmol) in dry dichloromethane (5 mL), was added triethylamine (2.32 mL, 16.66 mmol) followed by triphosgene (247 mg, 0.833 mmol) solution in dichloromethane (1 mL). The reaction mixture was stirred at room temperature for 1 h. To this mixture was then added tert-butyl 2-aminocyclohexylcarbamate (357 mg, 1.67 mmol) in dichloromethane (1 mL). The reaction mixture was stirred at room temperature for 4 h and concentrated. The residue was dissolved in ethyl acetate and washed with water (2×20 mL), brine (10 mL), dried and concentrated. The crude product was purified by flash column chromatography to afford the desired product as a mixture of cis and trans diastereomers (220 mg, 0.485 mmol, 58%). 1H NMR: 1.23-1.28 (m, 6H), 1.38 (s, 9H), 1.70-1.73 (m, 2H), 2.01-2.08 (m, 2H), 3.29-3.32 (m, 1H), 3.53-3.58 (m, 1H), 3.68 (s, 2H), 4.11-4.19 (m, 2H), 5.01 (d, 1H, J=8.8 Hz), 5.57 (d, 1H, J=8 Hz), 7.13 (d, 1H, J=8.4 Hz), 7.20 (d, 1H, J=6.8 Hz), 7.41 (s, 1H), 7.46 (s, 1H).

後処理

  1. stirringThe reaction mixture was stirred at room temperature for 4 h
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with water (2×20 mL), brine (10 mL)
  5. customdried
  6. concentrationconcentrated
  7. customThe crude product was purified by flash column chromatography

出典と根拠

ORDレコード
ord-45423655ff5b4e95a0d7ba40524bab19
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08722720B2

反応ノート

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