HCID 11564557、化合物 → HCID 58249836、化合物

HRID 1513539ノート

反応式

HRID 1513539 の反応式
[CH3:1][O:2][C:3](=[O:11])[CH2:4][C:5](=[O:10])[CH2:6][CH2:7][CH2:8][Cl:9].[H][H]>CO>[CH3:1][O:2][C:3](=[O:11])[CH2:4][CH:5]([OH:10])[CH2:6][CH2:7][CH2:8][Cl:9]

参加物

4

反応物 2

HCID 11564557HCID 11564557、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 58249836HCID 58249836、化合物収率 44%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 214.9 g portion of the above-mentioned crude 6-chloro-3-oxo-hexanoic acid methyl ester (1), Ru2Cl4-[(S)-Segphos]2(NEt)3 (60.7 mg, 0.0725×10−3 mol) and methanol (130 ml) were put into a 500 ml capacity autoclave and stirred with hydrogen (3 MPa) at 65 to 70° C. for 6 hours. After completion of the reaction, the solvent was evaporated under a reduced pressure using an evaporator, and then the residue was distilled under a reduced pressure (75 to 85° C./0.1 ton) to obtain 6-chloro-3-hydroxy-hexanoic acid methyl ester (2); 178.2 g {GC purity; 80.1%, pure amount; 142.7 g (0.790 mol, yield 44%/4-chlorobutanoic acid chloride)}.

後処理

  1. customAfter completion of the reaction
  2. customthe solvent was evaporated under a reduced pressure
  3. customan evaporator
  4. distillationthe residue was distilled under a reduced pressure (75 to 85° C./0.1 ton)

出典と根拠

ORDレコード
ord-7bd490fa9d134ed59a64309fbd876f3b
出典データセット
uspto-grants-2012_07
特許番号
US08217192B2

反応ノート

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