Hydrochloric Acid → 4-[6-(Difluoromethoxy)pyrazolo[1,5-a]pyrimidin-3-yl]-5-methylthiophene-2-carboxylic acid

HRID 1842607ノート

反応式

HRID 1842607 の反応式
C[O:2][C:3]([C:5]1[S:6][C:7]([CH3:23])=[C:8]([C:10]2[CH:11]=[N:12][N:13]3[CH:18]=[C:17]([O:19][CH:20]([F:22])[F:21])[CH:16]=[N:15][C:14]=23)[CH:9]=1)=[O:4].[OH-].[K+].CO.Cl>C1COCC1>[F:22][CH:20]([F:21])[O:19][C:17]1[CH:16]=[N:15][C:14]2[N:13]([N:12]=[CH:11][C:10]=2[C:8]2[CH:9]=[C:5]([C:3]([OH:4])=[O:2])[S:6][C:7]=2[CH3:23])[CH:18]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14797Potassium HydroxideHCID 68304950Methyl-4-[6-(difluoromethoxy)pyrazolo[1,5-a]pyrimidin-3-yl]-5-methylthiophene-2-carboxylate

生成物 1

HCID 683051734-[6-(Difluoromethoxy)pyrazolo[1,5-a]pyrimidin-3-yl]-5-methylthiophene-2-carboxylic acid収率 64.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
40 °C

実験手順

Methyl-4-[6-(difluoromethoxy)pyrazolo[1,5-a]pyrimidin-3-yl]-5-methylthiophene-2-carboxylate (0.916 g, 2.70 mmol) was dissolved in THF (4 mL). 1 M KOH in MeOH (12.0 mL, 12.0 mmol) was added and the reaction heated to 40° C. for 16 h. After the hydrolysis was complete, treated with 1N HCl and the resulting solids were filtered, washed with water and dried to afford the title compound (0.568 g, 1.75 mmol). LRMS (APCI) calc'd for (C13H9F2N3O3S) [M+H]+, 326.0; found 326.0.

後処理

  1. filtrationthe resulting solids were filtered
  2. washwashed with water
  3. customdried

出典と根拠

ORDレコード
ord-1e437e41b5dd443d90caf748b8be3afa
出典データセット
uspto-grants-2015_02
特許番号
US08946237B2

反応ノート

読み込み中…