Hydrochloric Acid → HCID 18996986、化合物

HRID 374640ノート

反応式

HRID 374640 の反応式
[CH:1]1[CH:6]=[C:5]([OH:7])[C:4]2[C:8]([C:10]3[C:15]([OH:16])=[CH:14][C:13]([CH2:17][OH:18])=[CH:12][C:11]=3[C:19](=[O:20])[C:3]=2[CH:2]=1)=[O:9].Cl>CS(C)=O.C(N(CC)CC)C>[OH:16][C:15]1[C:10]2[C:8](=[O:9])[C:4]3[C:3](=[CH:2][CH:1]=[CH:6][C:5]=3[OH:7])[C:19](=[O:20])[C:11]=2[CH:12]=[C:13]([CH:17]=[O:18])[CH:14]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 10207Aloe emodin

生成物 1

HCID 18996986HCID 18996986、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒2 回HCID 8471Triethylamine溶媒

実験手順

To aloe-emodin (5.0 g) in dry dimethyl sulphoxide (55 ml) and triethylamine (77 ml) was added a solution/suspension of sulphur trioxide-pyridine complex (29.4 g) in dry dimethyl sulphoxide (100 ml), dropwise with stirring, over 15 minutes. The addition was slightly exothermic and gave a dark brown solution, which was stirred at room temperature for 2-3 hours, then poured onto dilute hydrochloric acid (1000 ml, 0.5M), stirred for 15 minutes, then left to stand for 15 minutes. The suspension was filtered (slow), washed with water (400 ml) and pulled dry to leave a brown solid. Dried at 50° C. in a vacuum oven, m.p. 198°-200° C.

後処理

  1. additionThe addition
  2. customgave a dark brown solution, which
  3. stirringwas stirred at room temperature for 2-3 hours
  4. stirringstirred for 15 minutes
  5. waitleft
  6. waitto stand for 15 minutes
  7. filtrationThe suspension was filtered (slow)
  8. washwashed with water (400 ml)
  9. custompulled dry
  10. customto leave a brown solid
  11. customDried at 50° C. in a vacuum oven, m.p. 198°-200° C.

出典と根拠

ORDレコード
ord-13c599ecb62d487e8c0df00fb335ae89
出典データセット
uspto-grants-1996_01
特許番号
US05480873

反応ノート

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