Sodium Iodide → HCID 58079476, 화합물

HRID 562538

반응식

HRID 562538 반응식
[C:1]([OH:20])(=[O:19])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([OH:18])=[O:17].C(NC(C)C)(C)C.[CH3:28][O:29][C:30]1[CH:37]=[CH:36][C:33]([CH2:34]Cl)=[CH:32][CH:31]=1.[Na+].[I-]>CN1C(=O)CCC1.O>[CH3:28][O:29][C:30]1[CH:37]=[CH:36][C:33]([CH2:34][O:17][C:16](=[O:18])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][C:1]([OH:20])=[O:19])=[CH:32][CH:31]=1

참가 물질

7

반응물 4

HCID 5238Sodium IodideHCID 7912DiisopropylamineHCID 10459Hexadecanedioic acidHCID 699934-Methyloxybenzyl chloride

생성물 1

HCID 58079476HCID 58079476, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
80 °C

실험 절차

Hexadecandioic acid (2 g, 7 mmol) was dissolved in dry NMP (25 mL). Diisopropylamin (1.2 mL, 7 mmol) and 4-methoxybenzyl chloride (0.95 mL, 7 mmol) was added, followed by NaI (0.52 g, 3.5 mmol). The mixture was heated to 80° C. for 1 hour, poured into water (100 mL) and filtered. The precipate was washed with dichloromethane (150 mL), the dichoromethane phase was dried (Na2SO4) and solvent removed in vacuo to yield the crude product, which was recrystallized several times from heptane to yield hexadecanedioic acid mono-(4-methoxy-benzyl)ester.

후처리

  1. filtrationfiltered
  2. washThe precipate was washed with dichloromethane (150 mL)
  3. dry with materialthe dichoromethane phase was dried (Na2SO4) and solvent
  4. customremoved in vacuo
  5. customto yield the crude product, which
  6. customwas recrystallized several times from heptane

출처 및 근거

ORD 기록
ord-a807c31c1f234a7f857bc3f17d56ec3f
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067362B2

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