Methanol → methyl N-(2,6-dichlorobenzoyl)-4-iodo-L-phenylalaninate

HRID 1037817ノート

反応式

HRID 1037817 の反応式
[CH3:1]O.S(=O)(=O)(O)O.[Cl:8][C:9]1[CH:29]=[CH:28][CH:27]=[C:26]([Cl:30])[C:10]=1[C:11]([NH:13][C@H:14]([C:23]([OH:25])=[O:24])[CH2:15][C:16]1[CH:21]=[CH:20][C:19]([I:22])=[CH:18][CH:17]=1)=[O:12]>O>[CH3:1][O:24][C:23](=[O:25])[C@H:14]([CH2:15][C:16]1[CH:17]=[CH:18][C:19]([I:22])=[CH:20][CH:21]=1)[NH:13][C:11](=[O:12])[C:10]1[C:9]([Cl:8])=[CH:29][CH:28]=[CH:27][C:26]=1[Cl:30]

参加物

5

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 58018315HCID 58018315、化合物

生成物 1

HCID 59665509methyl N-(2,6-dichlorobenzoyl)-4-iodo-L-phenylalaninate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
40 °C

実験手順

Methanol (40 mL) and 0.98 mL of concentrated sulfuric acid were added to 8.0 g of Nα-(2,6-dichlorobenzoyl)-4-iodo-L-phenylalanine and the reaction was carried out for 4 hours while heating the reaction system at 40° C. After confirming the completion of the reaction, the reaction system was cooled to 10° C. and 20 mL of water was dropwise added to separate out solid. The solid thus precipitated was isolated through filtration under reduced pressure, washed with 40 mL of water and then dried at 70° C. under reduced pressure to thus give 7.40 g of the desired product as a solid.

後処理

  1. customthe completion of the reaction
  2. temperaturethe reaction system was cooled to 10° C.
  3. customto separate out solid
  4. customThe solid thus precipitated
  5. customwas isolated through filtration under reduced pressure
  6. washwashed with 40 mL of water
  7. dry with materialdried at 70° C. under reduced pressure to thus give 7.40 g of the desired product as a solid

出典と根拠

ORDレコード
ord-b6580e0b9fdd434fad8d5686965a6b2a
出典データセット
uspto-grants-2013_10
特許番号
US08546610B2

反応ノート

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