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Hydrochloric Acid → HCID 13536742, 화합물

HRID 464756
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반응식

HRID 464756 반응식
[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[O:11][C:10]([CH3:13])([CH3:12])[S:9][C:8]=2[CH:14]=1)([OH:3])=O.C(Cl)(=O)[C:16]([Cl:18])=O.Cl>CCOCC>[Cl:18][CH2:16][C:1]([C:4]1[CH:5]=[CH:6][C:7]2[O:11][C:10]([CH3:13])([CH3:12])[S:9][C:8]=2[CH:14]=1)=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 65578Oxalyl chlorideHCID 13536741HCID 13536741, 화합물

생성물 1

HCID 13536742HCID 13536742, 화합물수율 52%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture consisting of 10 g of 5-carboxy-2,2-dimethyl-1,3-benzoxathiole (IV), 10 g of oxalyl chloride and 20 ml of ether was boiled gently for 2 hours. The solution was cooled and evaporated and the residue (V) was added to an ether solution of diazomethane prepared from 25 g of N-nitroso-N-methyl urea. After stirring the mixture for 18 hours at room temperature the solution (VI) was acidified with methanolic hydrogen chloride and then evaporated to leave a solid residue which was recrystallized from ether/hexane to yield 6 g of 5-chloroacetyl-2,2-dimethyl-1,3-benzoxathiole (VII), m.p. 84°-86° C.

후처리

  1. temperatureThe solution was cooled
  2. customevaporated
  3. additionthe residue (V) was added to an ether solution of diazomethane
  4. customprepared from 25 g of N-nitroso-N-methyl urea
  5. customevaporated
  6. customto leave a solid residue which
  7. customwas recrystallized from ether/hexane

출처 및 근거

ORD 기록
ord-9bd27294aa1545dea12c4c02fecb08ff
출처 데이터셋
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04548951

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