Carbon Disulfide → ethyl hexahydro-4-isothiocyanato-1H-azepine-1-carboxylate

HRID 704712ノート

反応式

HRID 704712 の反応式
[C:1](=[S:3])=S.[NH2:4][CH:5]1[CH2:11][CH2:10][CH2:9][N:8]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:7][CH2:6]1>O1CCCC1>[N:4]([CH:5]1[CH2:11][CH2:10][CH2:9][N:8]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:7][CH2:6]1)=[C:1]=[S:3]

参加物

4

反応物 2

HCID 6348Carbon DisulfideHCID 15037323ethyl 4-aminohexahydro-1H-azepine-1-carboxylate

生成物 1

HCID 15037324ethyl hexahydro-4-isothiocyanato-1H-azepine-1-carboxylate収率 100%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred and cooled (-10° C.) mixture of 63 parts of carbon disulfide, 52.1 parts of N,N'-methanetetraylbis[cyclohexanamine] and 360 parts of tetrahydrofuran were added dropwise 46.9 parts of ethyl 4-aminohexahydro-1H-azepine-1-carboxylate. Upon complete addition, the reaction mixture was stirred for 2 hours at room temperature. The reaction mixture was evaporated and the residue was stirred in 2,2'-oxybispropane. The precipitate was filtered off and the filtrate was evaporated, yielding 70.75 parts (100%) of ethyl hexahydro-4-isothiocyanato-1H-azepine-1-carboxylate as a residue (interm. 29).

後処理

  1. temperaturecooled
  2. additionUpon complete addition
  3. stirringthe reaction mixture was stirred for 2 hours at room temperature
  4. customThe reaction mixture was evaporated
  5. stirringthe residue was stirred in 2,2'-oxybispropane
  6. filtrationThe precipitate was filtered off
  7. customthe filtrate was evaporated

出典と根拠

ORDレコード
ord-c0d906c3b4fc432dae52b96adb367275
出典データセット
uspto-grants-1991_01
特許番号
US04988689

反応ノート

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