Hydrochloric Acid → (S)-2-Amino-3-{(R)-2-[4-(3,4-dichloro-benzyloxy)-phenyl]-2,3-dihydro-benzo[1,4]dioxin-6-yl}-propionic acid methyl ester hydrochloride

HRID 879741ノート

反応式

HRID 879741 の反応式
[CH3:1][O:2][C:3](=[O:40])[C@@H:4]([NH:32]C(OC(C)(C)C)=O)[CH2:5][C:6]1[CH:31]=[CH:30][C:9]2[O:10][C@H:11]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH2:21][C:22]4[CH:27]=[CH:26][C:25]([Cl:28])=[C:24]([Cl:29])[CH:23]=4)=[CH:16][CH:15]=3)[CH2:12][O:13][C:8]=2[CH:7]=1.Cl>C(Cl)Cl>[ClH:28].[CH3:1][O:2][C:3](=[O:40])[C@@H:4]([NH2:32])[CH2:5][C:6]1[CH:31]=[CH:30][C:9]2[O:10][C@H:11]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH2:21][C:22]4[CH:27]=[CH:26][C:25]([Cl:28])=[C:24]([Cl:29])[CH:23]=4)=[CH:16][CH:15]=3)[CH2:12][O:13][C:8]=2[CH:7]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 58327327(S)-2-tert-Butoxycarbonylamino-3-{(R)-2-[4-(3,4-dichloro-benzyloxy)-phenyl]-2,3-dihydro-benzo[1,4]dioxin-6-yl}-propionic acid methyl ester

生成物 1

HCID 66719251(S)-2-Amino-3-{(R)-2-[4-(3,4-dichloro-benzyloxy)-phenyl]-2,3-dihydro-benzo[1,4]dioxin-6-yl}-propionic acid methyl ester hydrochloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

(S)-2-tert-Butoxycarbonylamino-3-{(R)-2-[4-(3,4-dichloro-benzyloxy)-phenyl]-2,3-dihydro-benzo[1,4]dioxin-6-yl}-propionic acid methyl ester (3.0 g) was dissolved in 60 mL DCM. 25 mL of 4N HCl (in dioxane) was added and the mixture stirred at room temperature for 2.5 hours. The mixture was concentrated and DCM added and mixture concentrated again. The resulting solid was dried under vacuum to provide 2.6 g. LCMS: m/z 489.

後処理

  1. concentrationThe mixture was concentrated
  2. additionDCM added
  3. concentrationmixture concentrated again
  4. customThe resulting solid was dried under vacuum
  5. customto provide 2.6 g

出典と根拠

ORDレコード
ord-e1b8d316744d4f57bd6b3403914d1a31
出典データセット
uspto-grants-2015_03
特許番号
US08987295B2

反応ノート

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