Hydrochloric Acid → HCID 178484724、化合物

HRID 16122

反応式

HRID 16122 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.[CH2:27]([N:29]([CH2:32]C)[CH2:30]C)C.ClC(Cl)([O:37]C(=O)OC(Cl)(Cl)Cl)Cl.Cl>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:27]([N:29]([CH3:32])[CH3:30])=[O:37])[CH2:22][CH2:21]2)[CH2:14][CH2:13]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471Triethylamine2 回HCID 94429TriphosgeneHCID 178478588HCID 178478588、化合物

生成物 1

HCID 178484724HCID 178484724、化合物収率 143.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

0.56 g (1.2 mmol) trans-4-{2-[4-(2,3-dichlorophenyl)-piperazin-1-yl]-ethyl}-cyclohexyl-amine trihydrochloride was suspended in dry dichloromethane (50 ml), triethylamine 0.77 ml, 6 mmol) was added and 0.13 g (0.44 mmol) triphosgene dissolved in dichloromethane was dropped in. After one hour stirring at room temperature dimetilamine hydrochloride (0.49 g, 6 mmol) followed by triethylamine (0.84 ml, 6 mmol) was added and the stirring was continued for 20 hours. The mixture was filtered, the filtrate washed with water, dried and evaporated in vacuo. Recrystallizing the product from methanol gave the title compound (0.27 g, 52%). Melting point: 212-4° C.

後処理

  1. additionwas dropped in
  2. additionwas added
  3. filtrationThe mixture was filtered
  4. washthe filtrate washed with water
  5. customdried
  6. customevaporated in vacuo
  7. customRecrystallizing the product from methanol

出典と根拠

ORDレコード
ord-258c082de91b464ba0230efdebd317cf
出典データセット
uspto-grants-2010_06
特許番号
US07737142B2

関連ノート

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