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Sodium Hydroxide → 4-({[(Tert-butoxy)carbonyl]amino}methyl)oxane-4-carboxylic acid

HRID 2047470
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인쇄 미리보기

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HRID 2047470 반응식
[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]1([C:16]([O:18]CC)=[O:17])[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+]>CO>[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]1([C:16]([OH:18])=[O:17])[CH2:11][CH2:12][O:13][CH2:14][CH2:15]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 67232523HCID 67232523, 화합물

생성물 1

HCID 170402064-({[(Tert-butoxy)carbonyl]amino}methyl)oxane-4-carboxylic acid수율 91.2%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
40 °C

실험 절차

To a solution of the compound (11.3 g) obtained in step 3 in methanol (190 mL) was added 2N aqueous sodium hydroxide solution (79 mL), and the mixture was stirred at 40° C. for 2 hr. The mixture was concentrated, diluted with ethyl acetate, and neutralized with 1N hydrochloric acid. The separated aqueous layer was extracted with ethyl acetate. The combined organic layer was dried, and concentrated under reduced pressure to give the title compound (9.3 g, 91%) as a white powder.

후처리

  1. concentrationThe mixture was concentrated
  2. additiondiluted with ethyl acetate
  3. extractionThe separated aqueous layer was extracted with ethyl acetate
  4. customThe combined organic layer was dried
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d85702c4879d4744a90d30e575f48e35
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08592454B2

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