Benzaldehyde → HCID 20528326, 화합물

HRID 67235

반응식

HRID 67235 반응식
[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]

참가 물질

8

반응물 5

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

생성물 1

HCID 20528326HCID 20528326, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-34472b1a55034bc2a3b0726c4608e611
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04344954

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