Water → HCID 19848014, 화합물

HRID 2351089노트

반응식

HRID 2351089 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 19848014HCID 19848014, 화합물수율 95.7%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-af2c0a3830d342dc9ac29171caab9c1d
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04871841

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