Hydrochloric Acid → 1-(2-Hydroxymethylbenzoyl)-2-methyl-4-(3-fluorophenyl)-3-thiosemicarbazide

HRID 1462994ノート

反応式

HRID 1462994 の反応式
[C:1]([C:5]1[CH:25]=[CH:24][CH:23]=[CH:22][C:6]=1[C:7]([NH:9][N:10]([CH3:21])[C:11]([NH:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=1)=[S:12])=[O:8])(OC)=[O:2].[BH4-].[Na+].O.Cl>C(O)C>[OH:2][CH2:1][C:5]1[CH:25]=[CH:24][CH:23]=[CH:22][C:6]=1[C:7]([NH:9][N:10]([CH3:21])[C:11]([NH:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=1)=[S:12])=[O:8]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 4311764Sodium borohydrideHCID 133374921-(2-Carbomethoxybenzoyl)-2-methyl-4-(3-fluorophenyl)-3-thiosemicarbazide

生成物 1

HCID 133374931-(2-Hydroxymethylbenzoyl)-2-methyl-4-(3-fluorophenyl)-3-thiosemicarbazide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1-(2-Carbomethoxybenzoyl)-2-methyl-4-(3-fluorophenyl)-3-thiosemicarbazide (7.2 g) was dissolved in ethanol (100 ml). The solution was cooled to below 10° and sodium borohydride (1.1 g) added. The mixture was then stirred at room temperature for 60 hours. Water was then added with production of an amorphous precipitate. Dilute hydrochloric acid was then added to the filtrate to bring it to pH 7 and further precipitate removed by filtration. The filtrate was thereupon acidified to yield the title product as a solid, m.p.136°-137°, yield 3.4 g.

後処理

  1. temperatureThe solution was cooled to below 10°
  2. customremoved by filtration

出典と根拠

ORDレコード
ord-a1c73654b16a47aeb68baa5084088678
出典データセット
uspto-grants-1984_07
特許番号
US04462821

反応ノート

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