Acetic Acid → 2-(Tritylthio)acetic acid

HRID 652747ノート

反応式

HRID 652747 の反応式
[SH:1][CH2:2][C:3]([OH:5])=[O:4].[C:6]1([C:12]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)O)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.C(O)(=O)C.B(F)(F)F.CCOCC>O>[C:6]1([C:12]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[S:1][CH2:2][C:3]([OH:5])=[O:4])[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 1133Thioglycolic AcidHCID 6457TriphenylcarbinolHCID 8000Boron trifluoride etherate

生成物 1

HCID 42453062-(Tritylthio)acetic acid収率 64,574.199%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

A mixture of distilled mercaptoacetic acid (20.87 g, 0.23 mmol), triphenylmethanol (60.0 g, 0.23 mol) and glacial acetic acid (200 ml) was heated to 70° C. Boron trifluoride etherate (32 ml, 0.25 mol) was added and the resulting brown mixture was stirred for 45 minutes at room temperature. The reaction mixture was then poured into water (500 ml), depositing a buff, granular solid which was filtered off, washed well with water then ether, and dried to give compound (V) (49.67 g, 67%). A further crop (12.27 g, 16%) was recovered from the ether washings, purified by recrystallization from benzene/hexanes. Both crops were homogeneous by TLC, mp 158.5°-160°.

後処理

  1. filtrationwas filtered off
  2. washwashed well with water
  3. dry with materialether, and dried

出典と根拠

ORDレコード
ord-72c720d74f6d464faa1d86a674086f23
出典データセット
uspto-grants-1987_06
特許番号
US04673562

反応ノート

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