Sulfur → HCID 12891716、化合物

HRID 1856566ノート

反応式

HRID 1856566 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9]([N:11]([CH2:26][CH3:27])[CH:12]1[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:14][CH2:13]1)=S.[S]>[Hg]=O.CO>[CH2:26]([N:11]([CH:12]1[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:14][CH2:13]1)[C:9]1[NH:8][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[N:1]=1)[CH3:27]

参加物

5

反応物 2

HCID 5362487SulfurHCID 12891715HCID 12891715、化合物

生成物 1

HCID 12891716HCID 12891716、化合物収率 43%

試薬・触媒・溶媒 2

HCID 30856Mercuric oxide触媒HCID 887Methanol溶媒

実験手順

A mixture of 39.8 parts of N-(2-aminophenyl)-N'-ethyl-N'-[I-(2-phenylethyl)-4-piperidinyl]thiourea, 15 parts of mercury oxide, 0.1 parts of sulfur and 400 parts of methanol is stirred and refluxed overnight. The reaction mixture is filtered hot over Hyflo and the filtrate is evaporated. The residue is crystallized from 4-methyl-2-pentanone. The product is filtered off and dried, yielding 14.5 parts (43%) of N-ethyl-N-[I-(2-phenylethyl)-4-piperidinyl]-1H-benzimidazol-2-amine; mp. 204.9° C.

後処理

  1. temperaturerefluxed overnight
  2. filtrationThe reaction mixture is filtered hot over Hyflo
  3. customthe filtrate is evaporated
  4. customThe residue is crystallized from 4-methyl-2-pentanone
  5. filtrationThe product is filtered off
  6. customdried

出典と根拠

ORDレコード
ord-1c6ea741abcc417cafc6a1c603e576f2
出典データセット
uspto-grants-1980_08
特許番号
US04219559

反応ノート

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