Carbon Disulfide → 1-(4-Isothiocyanatophenyl)-4-(4-methoxyphenyl)piperazine

HRID 1154729

反応式

HRID 1154729 の反応式
[C:1](=[S:3])=S.[CH3:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:17][CH2:16][N:15]([C:18]3[CH:23]=[CH:22][C:21]([NH2:24])=[CH:20][CH:19]=3)[CH2:14][CH2:13]2)=[CH:8][CH:7]=1.O(C(C)C)C(C)C>N1C=CC=CC=1>[N:24]([C:21]1[CH:20]=[CH:19][C:18]([N:15]2[CH2:16][CH2:17][N:12]([C:9]3[CH:10]=[CH:11][C:6]([O:5][CH3:4])=[CH:7][CH:8]=3)[CH2:13][CH2:14]2)=[CH:23][CH:22]=1)=[C:1]=[S:3]

参加物

5

反応物 3

HCID 6348Carbon DisulfideHCID 7914Diisopropyl EtherHCID 154406Benzenamine, 4-(4-(4-methoxyphenyl)-1-piperazinyl)-

生成物 1

HCID 155818991-(4-Isothiocyanatophenyl)-4-(4-methoxyphenyl)piperazine

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a stirred and cooled (ice-bath) mixture of 5 parts of N,N'-methanetetraylbis[cyclohexanamine], 25.2 parts of carbon disulfide and 40 parts of pyridine are added 6 parts of 4-[4-(4-methoxyphenyl)-1-piperazinyl]benzenamine and the whole is stirred first for 1 hour in an ice-bath and further for 2 hours at room temperature. 35 Parts of 2,2'-oxybispropane are added and the whole is stirred for 30 minutes. The precipitated product is filtered off and crystallized from 4-methyl-2-pentanone. The product is filtered off again and recrystallized from 1,4-dioxane, yielding 2.45 parts of 1-(4-isothiocyanatophenyl)-4-(4-methoxyphenyl)piperazine; mp. 180.6° C.

後処理

  1. temperaturecooled
  2. stirringthe whole is stirred first for 1 hour in an ice-bath and further for 2 hours at room temperature
  3. stirringthe whole is stirred for 30 minutes
  4. filtrationThe precipitated product is filtered off
  5. customcrystallized from 4-methyl-2-pentanone
  6. filtrationThe product is filtered off again
  7. customrecrystallized from 1,4-dioxane

出典と根拠

ORDレコード
ord-78468c47499e4d4badf7e5169b0757d3
出典データセット
uspto-grants-1984_12
特許番号
US04490530

関連ノート

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