Methanesulfonic Acid → MFCD01219577

HRID 2081659노트

반응식

HRID 2081659 반응식
CS(O)(=O)=O.[NH2:6][C:7](=[S:23])[NH:8][NH:9][C:10](=O)[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]>C1(C)C=CC=CC=1>[CH2:11]([C:10]1[S:23][C:7]([NH2:6])=[N:8][N:9]=1)[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 10730991HCID 10730991, 화합물

생성물 1

HCID 4319880MFCD01219577

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
0 °C

실험 절차

Methanesulfonic acid (6.26 g, 0.065 mol) was added in one portion to a slurry of the compound prepared in Step 1 above (11.9 g, 0.044 mol) in toluene (300 mL) at 0° C. After 5 minutes, the mixture was heated to reflux for 18 hours, allowed to cool to 0° C., filtered, and the residue washed with cold toluene (50 mL at 5° C). The solid was dried in vacuo, suspended in water (200 mL), and made basic with ammonium hydroxide (0.1M) while stirring vigorously. The resulting solid was filtered, washed with water, dried in vacuo to give 7.2 g of a white solid.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 18 hours
  3. filtrationfiltered
  4. washthe residue washed with cold toluene (50 mL at 5° C)
  5. customThe solid was dried in vacuo
  6. filtrationThe resulting solid was filtered
  7. washwashed with water
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-7cf2bc6ab274457bb0af7677d756c680
출처 데이터셋
uspto-grants-1993_02
특허 번호
US05185358

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