Dimethylcarbamoyl Chloride → HCID 178484724、化合物

HRID 16120

反応式

HRID 16120 の反応式
Cl.Cl.Cl.[Cl:4][C:5]1[C:10]([Cl:11])=[CH:9][CH:8]=[CH:7][C:6]=1[N:12]1[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][C@H:20]2[CH2:25][CH2:24][C@H:23]([NH2:26])[CH2:22][CH2:21]2)[CH2:14][CH2:13]1.C(N(CC)CC)C.[CH3:34][N:35]([CH3:39])[C:36](Cl)=[O:37]>ClCCl>[Cl:4][C:5]1[C:10]([Cl:11])=[CH:9][CH:8]=[CH:7][C:6]=1[N:12]1[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][C@H:20]2[CH2:25][CH2:24][C@H:23]([NH:26][C:36]([N:35]([CH3:39])[CH3:34])=[O:37])[CH2:22][CH2:21]2)[CH2:14][CH2:13]1

参加物

5

反応物 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 8471TriethylamineHCID 178478588HCID 178478588、化合物

生成物 1

HCID 178484724HCID 178484724、化合物収率 65%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1.39 g (3 mmol) trans-4-{2-[4-(2,3-dichlorophenyl)-piperazin-1-yl]-ethyl}-cyclohexyl-amine trihydrochloride was suspended in dichloromethane (100 ml), triethylamine (2.1 ml, 15 mmol) was added followed by 0.30 ml (3.3 mmol) N,N-dimethylcarbamoylchloride. The reaction mixture was stirred for 48 hours at room temperature, filtered. The filtrate was washed with water (2×20 ml), dried and evaporated in vacuo. Recrystallizing from methanol gave the title compound (0.83 g, 65%), melting at 212-4° C.

後処理

  1. filtrationfiltered
  2. washThe filtrate was washed with water (2×20 ml)
  3. customdried
  4. customevaporated in vacuo
  5. customRecrystallizing from methanol

出典と根拠

ORDレコード
ord-6738cef98f8145c9991bc3321e90ddd0
出典データセット
uspto-grants-2010_06
特許番号
US07737142B2

関連ノート

読み込み中…