2-Cyanoethanethioamide → HCID 178510482、化合物

HRID 2362819ノート

反応式

HRID 2362819 の反応式
[N:1]([CH2:4][CH2:5][O:6][C:7]1[CH:18]=[CH:17][C:10]([CH:11]=[C:12]([C:15]#[N:16])[C:13]#[N:14])=[CH:9][CH:8]=1)=[N+:2]=[N-:3].[C:19]([CH2:21][C:22]([NH2:24])=[S:23])#[N:20]>C(O)C>[NH2:16][C:15]1[C:12]([C:13]#[N:14])=[C:11]([C:10]2[CH:17]=[CH:18][C:7]([O:6][CH2:5][CH2:4][N:1]=[N+:2]=[N-:3])=[CH:8][CH:9]=2)[C:21]([C:19]#[N:20])=[C:22]([SH:23])[N:24]=1

参加物

4

反応物 2

HCID 14162772-CyanoethanethioamideHCID 86624335[4-(2-Azidoethoxy)benzylidene]malononitrile

生成物 1

HCID 178510482HCID 178510482、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2.39 g (9.98 mmol) of the compound from Example 37A and 2.50 g (24.92 mmol) of cyanothioacetamide in 100 ml of ethanol is stirred at +78° C. for 6 h. After cooling to RT and a further 12 h of standing without stirring, the reaction mixture is concentrated using a rotary evaporator. The residue is recrystallized from about 30 ml of ethanol. The resulting precipitate is filtered off with suction and washed twice with in each case 10 ml of methyl tert-butyl ether.

後処理

  1. concentrationthe reaction mixture is concentrated
  2. customa rotary evaporator
  3. customThe residue is recrystallized from about 30 ml of ethanol
  4. filtrationThe resulting precipitate is filtered off with suction
  5. washwashed twice with in each case 10 ml of methyl tert-butyl ether

出典と根拠

ORDレコード
ord-b01065bebd994833b94fcaac08b370c1
出典データセット
uspto-grants-2014_04
特許番号
US08691850B2

反応ノート

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