Ammonia → Methyl 3-(5-hydroxy-4,6,7-trimethyl-1,3-benzoxathiole-2-yl)propionate

HRID 2308864노트

반응식

HRID 2308864 반응식
COC(CCC([O:9][C:10]1[C:11]([CH3:27])=[C:12]([CH3:26])[C:13]2[O:17][CH:16]([CH2:18][CH2:19][C:20]([O:22][CH3:23])=[O:21])[S:15][C:14]=2[C:24]=1[CH3:25])=O)=O.N>CO>[OH:9][C:10]1[C:11]([CH3:27])=[C:12]([CH3:26])[C:13]2[O:17][CH:16]([CH2:18][CH2:19][C:20]([O:22][CH3:23])=[O:21])[S:15][C:14]=2[C:24]=1[CH3:25]

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 14802162Methyl 3-[5-(3-methoxycarbonylpropionyloxy)-4,6,7-trimethyl-1,3-benzoxathiole-2-yl]propionate

생성물 1

HCID 14802179Methyl 3-(5-hydroxy-4,6,7-trimethyl-1,3-benzoxathiole-2-yl)propionate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4.2 g of methyl 3-[5-(3-methoxycarbonylpropionyloxy)-4,6,7-trimethyl-1,3-benzoxathiole-2-yl]propionate (prepared as described in Example 31) were added to a mixture of 50 ml of methanol and 14 g of 28% w/v aqueous ammonia, and the mixture was reacted for 20 hours at room temperature. The volatile matter was then evaporated from the reaction mixture under reduced pressure, and ethyl acetate was added to the residue. The ethyl acetate solution was washed with water and dried over anhydrous sodium sulfate. The ethyl acetate was then distilled off under reduced pressure. The resulting residue was subjected to silica gel column chromatography, and the desired compound was obtained from the fraction eluted with a 20:1 by volume mixture of benzene and ethyl acetate.

후처리

  1. customthe mixture was reacted for 20 hours at room temperature
  2. customThe volatile matter was then evaporated from the reaction mixture under reduced pressure, and ethyl acetate
  3. additionwas added to the residue
  4. washThe ethyl acetate solution was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe ethyl acetate was then distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-4b047b0d27f14c91990cc076c92b4b99
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04691027

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