Sodium Hydroxide → 4-(Hydroxymethyl)benzoic acid

HRID 66228

반응식

HRID 66228 반응식
[OH:1][CH2:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9]C)=[O:8])=[CH:5][CH:4]=1.[OH-].[Na+]>O>[OH:1][CH2:2][C:3]1[CH:4]=[CH:5][C:6]([C:7]([OH:9])=[O:8])=[CH:11][CH:12]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 81325Methyl 4-(hydroxymethyl)benzoate

생성물 1

HCID 763604-(Hydroxymethyl)benzoic acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
20 °C

실험 절차

A mixture of Me pHMB (50.0 g., 0.30 mole) and 200 ml. of water containing sodium hydroxide (13.3 g., 0.33 mole) was refluxed for 3 hours. The colorless solution was filtered from a small amount (0.5 g.) of a gummy solid and extracted with methylene chloride (2 × 50 ml.). The aqueous portion was acidified with concentrated hydrochloric acid to give 37.0 g. of pHMBA: m.p. 180°-181° C. The filtrates were concentrated to 100 ml. at 100° C., cooled to 20° C., and filtered to give 6.7 g. of pHMBA (m.p. 181° C.). The combined yield of pHMBA was 43.7 g. (96%): silylation gc, 99.7% pHMBA.

후처리

  1. temperaturewas refluxed for 3 hours
  2. filtrationThe colorless solution was filtered from a small amount (0.5 g.) of a gummy solid
  3. extractionextracted with methylene chloride (2 × 50 ml.)
  4. customto give 37.0 g
  5. concentrationThe filtrates were concentrated to 100 ml
  6. filtrationfiltered
  7. customto give 6.7 g

출처 및 근거

ORD 기록
ord-6c6f3eac013e4b7aac9a479731454210
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04130719

연결된 노트

불러오는 중…