Acetic Acid → HCID 67165213、化合物

HRID 553315

反応式

HRID 553315 の反応式
[OH:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4][NH2:5].[CH3:10][O:11][C:12](=[O:22])[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([CH:20]=O)[CH:15]=1.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCl.CN1CCCC1=O>[CH3:10][O:11][C:12](=[O:22])[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([CH2:20][NH:5][CH2:4][C:3]2[CH:6]=[CH:7][CH:8]=[CH:9][C:2]=2[OH:1])[CH:15]=1

参加物

7

反応物 4

HCID 176Acetic AcidHCID 702672-(Aminomethyl)phenolHCID 5049666Sodium triacetoxyborohydrideHCID 11819590Methyl 2-(3-formylphenyl)acetate

生成物 1

HCID 67165213HCID 67165213、化合物収率 85.9%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

A mixture of 2-hydroxybenzylamine (407 mg) and (3-formylphenyl)acetic acid methyl ester (594 mg) in dichloromethane (10 mL) and 1-methyl-2-pyrrolidone (10 mL) was treated with acetic acid (333 mg) followed by sodium triacetoxyborohydride (1.41 g) and the whole stirred at room temperature for 18 hours. The reaction mixture was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate, the organic layer was washed twice with saturated aqueous brine before being separated, dried and evaporated under reduced pressure to yield the sub-titled compound (0.81 g).

後処理

  1. customThe reaction mixture was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate
  2. washthe organic layer was washed twice with saturated aqueous brine
  3. custombefore being separated
  4. customdried
  5. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-df1025b55b0e4d2da714fab1ad342103
出典データセット
uspto-grants-2011_05
特許番号
US07951954B2

関連ノート

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