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Hydrochloric Acid → HCID 68131886、化合物

HRID 1729711
ノート
印刷プレビュー

反応式

HRID 1729711 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 21500388HCID 21500388、化合物

生成物 1

HCID 68131886HCID 68131886、化合物

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-0f12b932248141b3a688cb956f34e98f
出典データセット
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03989714

反応ノート

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