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Hydrochloric Acid → HCID 178526005, 화합물

HRID 1380689
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HRID 1380689 반응식
[C:1]([CH2:8][N:9]1[C:13]([SH:14])=[N:12][N:11]=[N:10]1)([C:3]([O:5]CC)=[O:4])=[O:2].[OH-].[Na+].Cl>CO>[C:1]([CH2:8][N:9]1[C:13]([SH:14])=[N:12][N:11]=[N:10]1)([C:3]([OH:5])=[O:4])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 178473105HCID 178473105, 화합물

생성물 1

HCID 178526005HCID 178526005, 화합물수율 59.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 1-ethoxalylmethyl-1H-tetrazole-5-thiol (18.6 g) in methanol (186 ml) was added 1N aqueous solution of sodium hydroxide (172 ml) at room temperature and the mixture was stirred for 40 minutes. After adjusting to pH 7.5 with 10% hydrochloric acid, the solution was evaporated in vacuo to remove methanol and the remained aqueous solution was washed with ethyl acetate (100 ml). The aqueous solution was adjusted to pH 4.0 and washed again with ethyl acetate to remove impurities. The aqueous solution was adjusted to pH 2.5, and extracted with ethyl acetate, dried over magnesium sulfate and evaporated to give pale yellow powder of 1-oxalomethyl-1H-tetrazole-5-thiol (9.7 g), mp 140° to 150° C. (dec.).

후처리

  1. customthe solution was evaporated in vacuo
  2. customto remove methanol
  3. washthe remained aqueous solution was washed with ethyl acetate (100 ml)
  4. washwashed again with ethyl acetate
  5. customto remove impurities
  6. extractionextracted with ethyl acetate
  7. dry with materialdried over magnesium sulfate
  8. customevaporated

출처 및 근거

ORD 기록
ord-0fd3b5d239df4c618fa4b809ddcadba0
출처 데이터셋
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04582908

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