Benzenemethanamine, 2,5-dichloro- → 3-tert-Butylamino-4-(2,5-dichloro-benzylamino)-cyclobut-3-ene-1,2-dione

HRID 1956722ノート

反応式

HRID 1956722 の反応式
[Cl:1][C:2]1[CH:9]=[CH:8][C:7]([Cl:10])=[CH:6][C:3]=1[CH2:4][NH2:5].C([O:15][C:16]1[C:17](=[O:26])[C:18](=O)[C:19]=1[NH:20][C:21]([CH3:24])([CH3:23])[CH3:22])CCC>O1CCCC1>[C:21]([NH:20][C:19]1[C:16](=[O:15])[C:17](=[O:26])[C:18]=1[NH:5][CH2:4][C:3]1[CH:6]=[C:7]([Cl:10])[CH:8]=[CH:9][C:2]=1[Cl:1])([CH3:24])([CH3:22])[CH3:23]

参加物

4

反応物 2

HCID 457600Benzenemethanamine, 2,5-dichloro-HCID 178193893-Butoxy-4-tert-butylamino-cyclobut-3-ene-1,2-dione

生成物 1

HCID 178193743-tert-Butylamino-4-(2,5-dichloro-benzylamino)-cyclobut-3-ene-1,2-dione収率 52.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Employing the procedure of Example 2, Step 4, and a reaction period of 23 hours, 2,5-dichlorobenzylamine (0.88 g, 5 mmol) and 3-butoxy-4-tert-butylamino-cyclobut-3-ene-1,2-dione (1. 13 g, 5 mmol) in tetrahydrofuran (15 mL ) were converted to 1.52 g of a cream-colored solid. Recrystallization of this material from acetonitrile (twice) and from methanol provided 0.853 g of the tide compound as a white solid: mp 236° C. (softens 216° C.). MS (m/z) 326/328/330 (M+).

後処理

  1. customRecrystallization of this material from acetonitrile (twice) and from methanol

出典と根拠

ORDレコード
ord-049eba72c43d4e48bd0c64b358fa8146
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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