Water → 5-Amino-1-(2-carbamoyloxyethyl)pyrazole

HRID 1710286ノート

反応式

HRID 1710286 の反応式
C([NH:3][C:4]1[N:8]([CH2:9][CH2:10][OH:11])[N:7]=[CH:6][CH:5]=1)=O.ClS([N:16]=[C:17]=[O:18])(=O)=O.O.[OH-].[Na+]>C(#N)C>[NH2:3][C:4]1[N:8]([CH2:9][CH2:10][O:11][C:17](=[O:18])[NH2:16])[N:7]=[CH:6][CH:5]=1

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium Hydroxide2 回HCID 70918Chlorosulfonyl isocyanateHCID 150777375-Formamido-1-(2-hydroxyethyl)pyrazole

生成物 1

HCID 229167665-Amino-1-(2-carbamoyloxyethyl)pyrazole

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a suspension of 5-formamido-1-(2-hydroxyethyl)pyrazole (1 g) in acetonitrile (50 ml) was added dropwise chlorosulfonyl isocyanate (0.77 ml) at -15° C.~-20° C. The mixture was stirred for 3 hours under ice-cooling. To the reaction mixture was added water (1 ml) and kept to stand overnight. The solution was adjusted to pH 7.5 with 5N-sodium hydroxide solution and then adjusted to pH 8.5 with 1N-sodium hydroxide solution. The organic layer was separated and the aqueous layer was extracted with tetrahydrofuran. The extract and said organic layer were combined and dried over magnesium sulfate. The solvent was distilled off and the residue was crystallized from ethyl acetate to give 5-amino-1-(2-carbamoyloxyethyl)pyrazole (0.60 g).

後処理

  1. temperaturecooling
  2. waitto stand overnight
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted with tetrahydrofuran
  5. extractionThe extract
  6. dry with materialdried over magnesium sulfate
  7. distillationThe solvent was distilled off
  8. customthe residue was crystallized from ethyl acetate

出典と根拠

ORDレコード
ord-cc7f4d554ddf47d4b70cbef4cdaa8924
出典データセット
uspto-grants-1990_08
特許番号
US04952578

反応ノート

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