Hydrochloric Acid → HCID 20528325、化合物

HRID 67238

反応式

HRID 67238 の反応式
C(=O)C1C=CC(OC)=C(OC)C=1.FC1C=CC=CC=1C=O.[C-]#N.[K+].[CH3:25][O:26][C:27]1[CH:28]=[C:29]([C:35]([CH:37]([C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][C:40]=2[F:45])O)=[O:36])[CH:30]=[CH:31][C:32]=1[O:33][CH3:34].C1(C(C(C2C=CC=CC=2)O)=O)C=CC=CC=1.[NH:62]1[CH2:68][CH2:67][CH2:66][CH2:65][NH:64][C:63]1=[S:69].[ClH:70]>CC(C)=O.C(O)C>[ClH:70].[CH3:25][O:26][C:27]1[CH:28]=[C:29]([C:35]2([OH:36])[N:64]3[CH2:65][CH2:66][CH2:67][CH2:68][N:62]=[C:63]3[S:69][CH:37]2[C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][C:40]=2[F:45])[CH:30]=[CH:31][C:32]=1[O:33][CH3:34]

参加物

10

反応物 7

HCID 313Hydrochloric AcidHCID 8400BenzoinHCID 8419VeratraldehydeHCID 9032Potassium CyanideHCID 67970o-FluorobenzaldehydeHCID 7365891,3-Diazepane-2-thioneHCID 20528310HCID 20528310、化合物

生成物 1

HCID 20528325HCID 20528325、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 702Ethanol溶媒

実験手順

A mixture consisting of 16.6 g. of veratraldehyde, 12.5 g. of o-fluorobenzaldehyde, 8 g. of potassium cyanide, and 100 ml of 65% ethanol is reacted as described in Example 20, yielding 12.5 g. of 3,4-dimethoxy-2'-fluorobenzoin, m.p. 126°-128° C. A 5.8 g. portion of the benzoin derivative is converted to its methanesulfonate ester by the procedure of Example 20, giving 6.7 g. of the ester melting at 111°-113° C. 2.58 g. of the methanesulfonate ester, 0.91 g. of hexahydro-2H-1,3-diazepin-2-thione, and 55 ml. of acetone are mixed and left at room temperature for three days. 7 ml. of 2 N ethanolic hydrogen chloride are added, yielding 2.2 g. of the title compound, melting at 192°-194° C.

後処理

  1. customyielding 12.5 g
  2. customgiving 6.7 g
  3. customyielding 2.2 g

出典と根拠

ORDレコード
ord-2c17cee5591046558cc1b46ca1a3b269
出典データセット
uspto-grants-1982_08
特許番号
US04344954

関連ノート

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