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Hydrochloric Acid → HCID 68131886, 화합물

HRID 1729711
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HRID 1729711 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]2[CH:19]3[C:14]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=4)([CH2:15][CH2:16][CH2:17][CH2:18]3)[N:13](O)[CH2:12]2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[ClH:27]>[Zn].CO>[ClH:27].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]2[CH:19]3[C:14]([C:20]4[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=4)([CH2:15][CH2:16][CH2:17][CH2:18]3)[NH:13][CH2:12]2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 21500388HCID 21500388, 화합물

생성물 1

HCID 68131886HCID 68131886, 화합물

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 887Methanol용매

실험 절차

Zinc powder (20 g) was added to a stirred solution of 6.5 g (0.018 mole) of 3-(3,4-dimethoxyphenyl)-hexahydro-1-hydroxy-7a-phenylindoline, 150 ml of methanol and 150 ml of 1N hydrochloric acid and the mixture was maintained at reflux for 1/2 hour. The mixture was cooled, treated with excess of 10MKOH and extracted with two one liter portions of ether. The extracts were combined, dried (K2CO3) and filtered. Hydrogen chloride gas was bubbled into the ether solution until complete precipitation of the white salt; wt. 4.5 g (67.2%), mp 303°-305° C. Recrystallization from methanol-ether afforded pure white crystals, mp 303°-305° C.

후처리

  1. temperaturethe mixture was maintained
  2. temperatureat reflux for 1/2 hour
  3. temperatureThe mixture was cooled
  4. additiontreated with excess of 10MKOH and
  5. extractionextracted with two one liter portions of ether
  6. dry with materialdried (K2CO3)
  7. filtrationfiltered
  8. customHydrogen chloride gas was bubbled into the ether solution until complete precipitation of the white salt
  9. customRecrystallization from methanol-ether afforded pure white crystals, mp 303°-305° C.

출처 및 근거

ORD 기록
ord-0f12b932248141b3a688cb956f34e98f
출처 데이터셋
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03989714

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