Triethylamine → HCID 21187839、化合物

HRID 356902

反応式

HRID 356902 の反応式
[CH:1]1([O:6][C:7]2[CH:8]=[C:9]([CH:11]=[CH:12][C:13]=2[O:14][CH3:15])[NH2:10])[CH2:5][CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[Cl:23][C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([Cl:30])[C:25]=1[N:31]=[C:32]=[O:33]>ClCCl>[Cl:23][C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([Cl:30])[C:25]=1[NH:31][C:32]([NH:10][C:9]1[CH:11]=[CH:12][C:13]([O:14][CH3:15])=[C:7]([O:6][CH:1]2[CH2:2][CH2:3][CH2:4][CH2:5]2)[CH:8]=1)=[O:33]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 6045371,3-Dichloro-2-isocyanatobenzeneHCID 27793343-(Cyclopentyloxy)-4-methoxyaniline

生成物 1

HCID 21187839HCID 21187839、化合物収率 56%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A stirred solution of 3-cyclopentyloxy-4-methoxyaniline (1 g) and triethylamine (0.69 mL) in dry dichloromethane (20 mL) is treated dropwise at 0°-5° C. with a solution of 2,6-dichlorophenyl isocyanate (0.9 g) in dry dichloromethane (10 mL). The resulting mixture is stirred for 30 minutes at this temperature and then for 6 hours at room temperature. The precipitate which forms is collected and stirred with isopropanol (50 mL), with ice cooling. The resulting solid is collected and dried, to give N-(2,6-dichlorophenyl)-N'-(3-cyclopentyloxy-4-methoxyphenyl)urea (1.06 g), m.p. 203°-204° C. [Elemental analysis: C,57.2; H,5.0; N,7.0; Cl,18.2%; calculated: C,57.7; H,5.1; N,7.1; Cl,18.0%].

後処理

  1. waitfor 6 hours at room temperature
  2. customThe precipitate which forms is collected
  3. stirringstirred with isopropanol (50 mL), with ice cooling
  4. customThe resulting solid is collected
  5. customdried

出典と根拠

ORDレコード
ord-b8fe25528be34bf69fb2ac3fb8c32d8c
出典データセット
uspto-grants-1998_11
特許番号
US05840724

関連ノート

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