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

HRID 877950노트

반응식

HRID 877950 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].C(=O)([O-])[O-].[K+].[K+]>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

5

반응물 3

HCID 8007ButylamineHCID 11430Potassium CarbonateHCID 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

반응 조건

온도
42.5 °C

실험 절차

A mixture of tert-butyl 2-((4R,6S)-6-(hydroxymethyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate (10 grams), methanol (80 ml), n-butyl amine (20 ml) and potassium carbonate (10.6 grams) was heated to 40-45° C. and stirred up to completion of the reaction. The reaction mixture was distilled under reduced pressure and methylene chloride (100 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. distillationThe reaction mixture was distilled under reduced pressure and methylene chloride (100 ml)
  2. additionwas added to the obtained residue at 25-30° C.
  3. stirringstirred for 15 minutes
  4. filtrationThe unwanted solid was filtered off
  5. distillationthe filtrate was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-b273afee20fe4c5db7c346d0d7b47bfd
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987444B2

반응 노트

불러오는 중…