Water → HCID 19848014、化合物

HRID 2351089ノート

反応式

HRID 2351089 の反応式
[O:1]=[C:2]1[NH:7][CH2:6][CH2:5][CH2:4][N:3]1[NH:8][C:9](=[O:18])[O:10][CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.ClS([N:23]=[C:24]=[O:25])(=O)=O.O>C(OCC)(=O)C>[O:1]=[C:2]1[N:3]([NH:8][C:9]([O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[O:18])[CH2:4][CH2:5][CH2:6][N:7]1[C:24]([NH2:23])=[O:25]

参加物

5

反応物 3

HCID 962WaterHCID 70918Chlorosulfonyl isocyanateHCID 54188774(Tetrahydro-2-oxo-1(2H)-pyrimidinyl)carbamic acid, phenylmethyl ester

生成物 1

HCID 19848014HCID 19848014、化合物収率 95.7%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a suspension of (tetrahydro-2-oxo-1(2H)-pyrimidinyl)carbamic acid, phenylmethyl ester (35.5 g, 135.9 mmol) in 500 ml ethyl acetate, chlorosulfonyl isocyanate (24.0 g, 169.9 mmol) was added. The resulting solution was stirred for one hour and hydrolyzed by adding 175 ml water. The phases were separated, the organic phase washed with water and brine and dried over magnesium sulfate. Evaporation of the solvent and trituration of the residue with ether yielded 38.0 g of the desired product, melting point 135.6° C.

後処理

  1. additionwas added
  2. customThe phases were separated
  3. washthe organic phase washed with water and brine
  4. dry with materialdried over magnesium sulfate
  5. customEvaporation of the solvent and trituration of the residue with ether

出典と根拠

ORDレコード
ord-af2c0a3830d342dc9ac29171caab9c1d
出典データセット
uspto-grants-1989_10
特許番号
US04871841

反応ノート

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