Benzaldehyde → HCID 20528326、化合物

HRID 67235

反応式

HRID 67235 の反応式
[C-]#N.[K+].C(=O)C1C=CC=CC=1.S1C=CC=C1[C:17]([C:25]([C:27]([OH:39])([C:34]1[S:35][CH:36]=[CH:37][CH:38]=1)C1C=CC=CC=1)=O)(O)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20]C=1.[CH3:40][S:41](Cl)(=[O:43])=[O:42].[NH:45]1[CH2:51][CH2:50][CH2:49][CH2:48][NH:47][C:46]1=[S:52]>CC(C)=O.C(O)C>[CH3:40][S:41]([O:39][C:27]1([C:34]2[S:35][CH:36]=[CH:37][CH:38]=2)[N:47]2[CH2:48][CH2:49][CH2:50][CH2:51][N:45]=[C:46]2[S:52][CH:25]1[C:17]1[CH:18]=[CH:23][CH:22]=[CH:21][CH:20]=1)(=[O:43])=[O:42]

参加物

8

反応物 5

HCID 240BenzaldehydeHCID 9032Potassium CyanideHCID 31297Methanesulfonyl chlorideHCID 7365891,3-Diazepane-2-thioneHCID 540020012-Thienyl-alpha-hydroxybenzyl ketone

生成物 1

HCID 20528326HCID 20528326、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 702Ethanol溶媒

実験手順

A mixture of 9.2 ml. of thiophene-2-carboxyaldehyde, 8 g. of potassium cyanide and 10.1 ml. of benzaldehyde in 100 ml. of 65% ethanol is reacted as described in Example 20, giving 6.2 g. of 2-thienyl-α-hydroxybenzyl ketone. A 4.36 g. portion of this ketone is reacted with methanesulfonyl chloride as described in Example 20, giving 3.2 g. of the methanesulfonate ester. A 2.64 g. portion of this ester and 1.30 g. of hexahydro-2H-1,3-diazepine-2-thione in 100 ml. of acetone are allowed to stand 48 hours, the solid is collected, washed with ether and dried in vacuo, giving 2.8 g. of the desired product, m.p. 149°-151° C.

後処理

  1. additionA mixture of 9.2 ml
  2. customgiving 6.2 g
  3. customgiving 3.2 g
  4. customthe solid is collected
  5. washwashed with ether
  6. customdried in vacuo
  7. customgiving 2.8 g

出典と根拠

ORDレコード
ord-34472b1a55034bc2a3b0726c4608e611
出典データセット
uspto-grants-1982_08
特許番号
US04344954

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