Ammonia → HCID 22457552, 화합물

HRID 2184709노트

반응식

HRID 2184709 반응식
C([O:4][CH2:5][CH2:6][C:7]1[C:16]2[C:11](=[C:12]([N+:17]([O-:19])=[O:18])[CH:13]=[CH:14][CH:15]=2)[C:10]([S:20](Cl)(=[O:22])=[O:21])=[CH:9][CH:8]=1)(=O)C.[NH3:24].CO>>[OH:4][CH2:5][CH2:6][C:7]1[C:16]2[C:11](=[C:12]([N+:17]([O-:19])=[O:18])[CH:13]=[CH:14][CH:15]=2)[C:10]([S:20]([NH2:24])(=[O:22])=[O:21])=[CH:9][CH:8]=1

참가 물질

4

반응물 3

HCID 222AmmoniaHCID 887MethanolHCID 22457564HCID 22457564, 화합물

생성물 1

HCID 22457552HCID 22457552, 화합물

실험 절차

Solid 4-(2-acetoxy-ethyl)-8-nitro-naphthalene-1-sulfonyl chloride (39.64 g, 111 mmol) was added to an ice-cold, 6.8 M solution of ammonia in methanol (408 mL, 277 mmol). The cooling bath was removed, the reaction flask was stoppered, and the reaction was stirred at room temperature. After 4 days, the dark amber solution was concentrated under vacuum to a dark gum. The residue was triturated vigorously shaken with water (300 mL) to give a solid which was washed with water (150 mL) then ether (150 mL) and dried under vacuum. The resulting brown solid was recrystallized from isopropanol (300 mL) to afford 4-(2-hydroxy-ethyl)-8-nitro-naphthalene-1-sulfonamide (27.79 g) as tan flakes.

후처리

  1. customThe cooling bath was removed
  2. concentrationthe dark amber solution was concentrated under vacuum to a dark gum
  3. customThe residue was triturated vigorously
  4. stirringshaken with water (300 mL)
  5. customto give a solid which
  6. washwas washed with water (150 mL)
  7. dry with materialether (150 mL) and dried under vacuum
  8. customThe resulting brown solid was recrystallized from isopropanol (300 mL)

출처 및 근거

ORD 기록
ord-b4ed599a70f349f79f8cd3374997e2d4
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06399597B1

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