2,3-Dichlorobenzylamine → 3-(t-Butylamino)-4-(2,3-dichloro-benzylamino)-cyclobut-3-ene-1,2-dione

HRID 1956732ノート

反応式

HRID 1956732 の反応式
C(O[C:6]1[C:7](=[O:16])[C:8](=[O:15])[C:9]=1[NH:10][C:11]([CH3:14])([CH3:13])[CH3:12])CCC.[Cl:17][C:18]1[C:25]([Cl:26])=[CH:24][CH:23]=[CH:22][C:19]=1[CH2:20][NH2:21]>O1CCCC1>[C:11]([NH:10][C:9]1[C:8](=[O:15])[C:7](=[O:16])[C:6]=1[NH:21][CH2:20][C:19]1[CH:22]=[CH:23][CH:24]=[C:25]([Cl:26])[C:18]=1[Cl:17])([CH3:12])([CH3:13])[CH3:14]

参加物

4

反応物 2

HCID 5876252,3-DichlorobenzylamineHCID 178193893-Butoxy-4-tert-butylamino-cyclobut-3-ene-1,2-dione

生成物 1

HCID 178193403-(t-Butylamino)-4-(2,3-dichloro-benzylamino)-cyclobut-3-ene-1,2-dione収率 89.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Tetrahydrofuran (12 mL), 3-butoxy-4-tert-butylamino-cyclobut-3-ene-1,2-dione (1.13 g, 5.0 mmol, Example 1), and 2,3-dichlorobenzylamine (0.88 g, 5.0 mmol) were stirred together at room temperature for 64 hours. After removal of solvent, trituation of the residue with diethyl ether and drying gave 1.46 g of a white solid. Four recrystallizations of this crude product from acetonitrile provided 0.927 g of the title compound as a white solid: mp 237°-243° C. (dec). MS (m/z) 327 ([M+H]+).

後処理

  1. customAfter removal of solvent, trituation of the residue with diethyl ether
  2. customdrying

出典と根拠

ORDレコード
ord-51accb6a80204638ada9d6fca9847a9b
出典データセット
uspto-grants-1998_07
特許番号
US05780505

反応ノート

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