Hydrochloric Acid → HCID 765906、化合物

HRID 988615ノート

反応式

HRID 988615 の反応式
[C:1]([C:5]1[CH:23]=[CH:22][C:8]([C:9]([NH:11][C:12]2[CH:21]=[CH:20][CH:19]=[CH:18][C:13]=2[C:14]([O:16]C)=[O:15])=[O:10])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].C1COCC1.[OH-].[Li+].Cl>CO>[C:1]([C:5]1[CH:23]=[CH:22][C:8]([C:9]([NH:11][C:12]2[CH:21]=[CH:20][CH:19]=[CH:18][C:13]=2[C:14]([OH:16])=[O:15])=[O:10])=[CH:7][CH:6]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 772645HCID 772645、化合物

生成物 1

HCID 765906HCID 765906、化合物収率 98%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A stirring solution of methyl 2-(4-tert-butylbenzoylamino)benzoate (10.4 g, 33.4 mmol) and THF (200 mL) was treated with 1 M aqueous lithium hydroxide (40 mL) and methanol (80 mL). After stirring over night at room temperature, the mixture was treated with 1 M aqueous HCl (40 mL) and the solvent was removed in vacuo. The residue was partitioned between ethyl acetate (400 mL) and brine (100 mL). The organic phase was separated, then dried with MgSO4, filtered and concentrated in vacuo to give 9.69 g (98%) of a white powder.

後処理

  1. customthe solvent was removed in vacuo
  2. customThe residue was partitioned between ethyl acetate (400 mL) and brine (100 mL)
  3. customThe organic phase was separated
  4. dry with materialdried with MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-ddb8284d961049ada90392b88199078c
出典データセット
uspto-grants-2003_10
特許番号
US06635657B1

反応ノート

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