Acetic Acid → 3-(Cyclopropylmethoxy)-4-(difluoromethoxy)benzoic Acid

HRID 631781ノート

反応式

HRID 631781 の反応式
[CH:1]1([CH2:4][O:5][C:6]2[CH:7]=[C:8]([CH:11]=[CH:12][C:13]=2[O:14][CH:15]([F:17])[F:16])[CH:9]=[O:10])[CH2:3][CH2:2]1.C(O)(=[O:20])C.S(=O)(=O)(O)N.[Cl-].[Na+]>O>[CH:1]1([CH2:4][O:5][C:6]2[CH:7]=[C:8]([CH:11]=[CH:12][C:13]=2[O:14][CH:15]([F:16])[F:17])[C:9]([OH:20])=[O:10])[CH2:3][CH2:2]1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 5234Sodium ChlorideHCID 5987Sulfamic AcidHCID 189736983-(Cyclopropylmethoxy)-4-(difluoromethoxy)benzaldehyde

生成物 1

HCID 23940063-(Cyclopropylmethoxy)-4-(difluoromethoxy)benzoic Acid収率 85%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
7.5 °C

実験手順

40 g of 3-(cyclopropylmethoxy)-4-(difluoromethoxy)-benzaldehyde 160 mL of glacial acetic acid and 32.0 g of sulphamic acid (2.0 eq) were loaded in a reactor. The mixture was cooled at 5-10° C. and the temperature was not allowed to exceed 20° C., adding slowly a previously prepared solution of 44.77 g of sodium chloride and 61 mL of deionised water. After the addition, the reaction was kept for 1 hour at 15-20° C. 450 mL of deionised water was loaded and then it was cooled at 0-5° C. and kept for 1 h at this temperature. The solid was filtered and washed four times with 200 mL of deionised water. The product was dried for 15 h at 40° C., obtaining 36 g (yield 85%) of 3-(cyclopropylmethoxy)-4-(difluoromethoxy)-benzoic acid (II) as solid.

後処理

  1. customto exceed 20° C.
  2. additionAfter the addition
  3. temperatureit was cooled at 0-5° C.
  4. waitkept for 1 h at this temperature
  5. filtrationThe solid was filtered
  6. washwashed four times with 200 mL of deionised water
  7. customThe product was dried for 15 h at 40° C.

出典と根拠

ORDレコード
ord-137d8b51a49d4c059e07ba72f7b8b027
出典データセット
uspto-grants-2016_04
特許番号
US09321726B2

反応ノート

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