Methanesulfonic Acid → MFCD01219577

HRID 2081659ノート

反応式

HRID 2081659 の反応式
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]

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 10730991HCID 10730991、化合物

生成物 1

HCID 4319880MFCD01219577

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7cf2bc6ab274457bb0af7677d756c680
出典データセット
uspto-grants-1993_02
特許番号
US05185358

反応ノート

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