Potassium Hydroxide → 2-(8-benzylamino-6,7,8,9-tetrahydro-5H-benzocyclohepten-2-yloxy)-2-methylpropionic acid

HRID 274046ノート

反応式

HRID 274046 の反応式
[CH2:1]([NH:8][CH:9]1[CH2:15][C:14]2[CH:16]=[C:17]([OH:20])[CH:18]=[CH:19][C:13]=2[CH2:12][CH2:11][CH2:10]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH2:21].Cl[C:23](Cl)(Cl)[C:24]([CH3:27])(O)[CH3:25].[OH-:30].[K+]>CC(C)=O>[CH2:1]([NH:8][CH:9]1[CH2:15][C:14]2[CH:16]=[C:17]([O:20][C:24]([CH3:27])([CH3:25])[C:23]([OH:30])=[O:21])[CH:18]=[CH:19][C:13]=2[CH2:12][CH2:11][CH2:10]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 122198322-Propanol, 1,1,1-trichloro-2-methyl-, hydrateHCID 18007284HCID 18007284、化合物

生成物 1

HCID 200947372-(8-benzylamino-6,7,8,9-tetrahydro-5H-benzocyclohepten-2-yloxy)-2-methylpropionic acid収率 39.8%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a mixture of 8-benzylamino-6,7,8,9-tetrahydro-5H-benzocyclohepten-2-ol (970 mg) and 1,1,1-trichloro-2-methyl-2-propanol hydrate (1.28 g) in acetone (30 ml) was added portionwise powder KOH (1.71 g) and the mixture was stirred for 20 hours at ambient temperature. After the solvent was evaporated in vacuo, the residue was poured into 1N sodium hydroxide (30 ml) and washed with diethyl ether. The pH of the aqueous layer was adjusted to 6.0 with 3N hydrochloric acid. The precipitates were filtered off. The filtrate was concentrated in vacuo and water was added to the residue. The resulting precipitates were collected by filtration and dried to give 2-[8-benzylamino-6,7,8,9-tetrahydro-5H-benzocyclohepten-2-yloxy]-2-methylpropionic acid (0.51 g).

後処理

  1. customAfter the solvent was evaporated in vacuo
  2. additionthe residue was poured into 1N sodium hydroxide (30 ml)
  3. washwashed with diethyl ether
  4. filtrationThe precipitates were filtered off
  5. concentrationThe filtrate was concentrated in vacuo and water
  6. additionwas added to the residue
  7. customThe resulting precipitates
  8. filtrationwere collected by filtration
  9. customdried

出典と根拠

ORDレコード
ord-74828932c7fb4ca9b27ccec206303d0d
出典データセット
uspto-grants-1995_02
特許番号
US05387710

反応ノート

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