Butylamine → N-butyl-2-((4R,6S)-6-(hydroxymethyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetamide

HRID 877951노트

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HRID 877951 반응식
[OH:1][CH2:2][C@H:3]1[O:8][C:7]([CH3:10])([CH3:9])[O:6][C@@H:5]([CH2:11][C:12]([O:14]C(C)(C)C)=O)[CH2:4]1.[CH2:19]([NH2:23])[CH2:20][CH2:21][CH3:22]>CO>[CH2:19]([NH:23][C:12](=[O:14])[CH2:11][C@H:5]1[CH2:4][C@@H:3]([CH2:2][OH:1])[O:8][C:7]([CH3:9])([CH3:10])[O:6]1)[CH2:20][CH2:21][CH3:22]

참가 물질

4

반응물 2

HCID 8007ButylamineHCID 9816650tert-Butyl 2,4-dideoxy-3,5-O-(1-methylethylidene)-D-erythro-hexonate

생성물 1

HCID 53339170N-butyl-2-((4R,6S)-6-(hydroxymethyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetamide

시약·촉매·용매 1

HCID 887Methanol용매

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온도
65 °C

실험 절차

Mixture of tert-butyl 2-((4R,6S)-6-(hydroxymethyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate (50 grams), methanol (300 ml) and n-butyl amine (200 ml) was heated to 60-70° C. under nitrogen pressure and stirred. After the completion of the reaction, distilled off the reaction mixture completely followed by co-distillation with methylene chloride at below 55° C. Methylene chloride (500 ml) was added to the obtained residue at 25-30° C. and stirred for 15 minutes. The unwanted solid was filtered off and the filtrate was distilled off under reduced pressure to get the title compound.

후처리

  1. customAfter the completion of the reaction
  2. distillationdistilled off the reaction mixture
  3. customcompletely followed by co-distillation with methylene chloride at below 55° C
  4. additionMethylene chloride (500 ml) was added to the obtained residue at 25-30° C.
  5. stirringstirred for 15 minutes
  6. filtrationThe unwanted solid was filtered off
  7. distillationthe filtrate was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-d2d5b4cdaaf74778a8698f5a8416efec
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987444B2

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