Water → Carbamic acid, (6-hydroxyhexyl)-, phenylmethyl ester

HRID 465139

반응식

HRID 465139 반응식
[CH2:1]([O:8][C:9]([O:11]N1C(=O)CCC1=O)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][OH:26].O>O1CCCC1.CO>[CH2:1]([O:8][C:9]([NH:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][OH:26])=[O:11])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 199606-Amino-1-hexanolHCID 83172Benzyl succinimido carbonate

생성물 1

HCID 4184071Carbamic acid, (6-hydroxyhexyl)-, phenylmethyl ester

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 32 g of N-benzyloxycarbonyloxysuccinimide in 100 ml of tetrahydrofuran is reacted with 15 g of 6-amino-1-hexanol in 30 ml of 50% methanol:tetrahydrofuran. The reaction mixture is stirred overnight at room temperature, and poured into water. The resulting mixture is extracted with methylene chloride and the organic layer is washed with sodium chloride solution, dried over anhydrous magnesium sulfate. The magnesium sulfate is filtered and the solvent is removed by evaporation. The product is recrystallized from ethyl acetate/ether to provide N-(benzyloxycarbonyl)-6-amino-1-hexanol, mp 81.5°-83° C. having the following formula: ##STR32##

후처리

  1. extractionThe resulting mixture is extracted with methylene chloride
  2. washthe organic layer is washed with sodium chloride solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationThe magnesium sulfate is filtered
  5. customthe solvent is removed by evaporation
  6. customThe product is recrystallized from ethyl acetate/ether

출처 및 근거

ORD 기록
ord-adac9afde4b44914890d098de66957e8
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04550163

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