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Acetic Anhydride → HCID 10909996, 화합물

HRID 1670354
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HRID 1670354 반응식
[CH:1]1([C@H:7]([OH:9])[CH3:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:10](OC(=O)C)(=[O:12])[CH3:11]>C1(C)C=CC(S(O)(=O)=O)=CC=1>[C:10]([O:9][C@@H:7]([CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)[CH3:8])(=[O:12])[CH3:11]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 10290808(alphaR)-alpha-Methylcyclohexanemethanol

생성물 1

HCID 10909996HCID 10909996, 화합물수율 99.9%

시약·촉매·용매 1

HCID 6101p-Toluenesulfonic acid촉매

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온도
35 °C

실험 절차

A 2 L reaction flask was charged with (R)-1-cyclohexylethanol (980 g, synthesized as above), acetic anhydride (1 Kg), and p-toluene sulphonic acid (0.4 g), and heated at 30-40° C. for 6 hours. The reaction mixture was then transferred into a separatory funnel and washed twice in 200 mL water followed by once in 200 mL 10% sodium hydroxide (aOH). The resulted organic layer was distilled at 5-10 mmHg to provide (R)-1-cyclohexylethyl acetate (1.3 Kg) (optical rotation: [α]D+2.59°; optical purity: 80.5% ee ).

후처리

  1. customA 2 L reaction flask
  2. customThe reaction mixture was then transferred into a separatory funnel
  3. washwashed twice in 200 mL water
  4. distillationThe resulted organic layer was distilled at 5-10 mmHg

출처 및 근거

ORD 기록
ord-b3ed9727a9794156869c102697b7adbd
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07993633B2

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